3EPA
United States
Environmental Protection
Agency
Great Lakes
National Program Office
77 West Jackson Boulevard
Chicago, Illinois 60604
EPA 905-R93-005
December 1993
Assessment and
Remediation
Of Contaminated Sediments
(ARCS) Program
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION FOR
THE TREATMENT OF BUFFALO
RIVER SEDIMENTS
•) United States Areas of Concern
P ARCS Priority Areas of Concern
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Pilot-Scale Demonstration of Thermal Desorption for the
Treatment of Buffalo River Sediments
Final Report
Prepared by
US Army Engineer District, Buffalo
For the
Assessment and Remediation of Contaminated Sediments (ARCS) program
U.S. Environmental Protection Agency
Great Lakes National Program Office
Chicago, Illinois
U.S. Environmental Protection
R^ion 5.Library (PI.-12J)
/'/ \V-ci Jackson Boulevard. I2ttl
Chicago, JL 60604-3590
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PILOT-SCALE DEMONSTRATION OF THERMAL DESORPTION FOR THE
TREATMENT OF BUFFALO RIVER SEDIMENTS
ABSTRACT
This report presents the results of a pilot scale
demonstration to remediate contaminated sediments from the
Buffalo River. A thermal desorption unit was evaluated for its
effectiveness in remediating Buffalo River sediments contaminated
with polycyclic aromatic hydrocarbons (PAHs). Sediments were
processed at various water contents, thermal unit residence
times, and temperatures to evaluate the effect of these process
variables on treatment efficiency and materials handling. A
portion of the residual solids from the thermal treatment process
was mixed with various proportions of Portland cement to evaluate
the ability of one solidification/stabilization process to bind
metal contaminants.
With sediments remaining in the thermal desorption unit from 30
to 90 minutes and sediment temperatures reaching 300 to 480°F;
43.2 to 97.9 percent of total PAHs were removed while 9.1 to 100
percent of total PCBs (Aroclors 1248 and 1254) were removed.
Although this thermal process had little effect on most metals,
16.7 to 100 percent of mercury was removed from sediments during
processing. Removal rates for constituents of concern did not
correlate well with treatment times or temperatures.
This paper has been reviewed in accordance with the U.S.
Environmental Protection Agency's peer and administrative review
policies and approved for presentation and publication.
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FINAL REPORT
PILOT-SCALE DEMONSTRATION OF THERMAL DESORPTION FOR THE
TREATMENT OF BUFFALO RIVER SEDIMENTS
TABLE OF CONTENTS
Paragraph Page
ABSTRACT i
TABLE OF CONTENTS ii
TABLES v
FIGURES vii
ABBREVIATIONS AND SYMBOLS viii
1 INTRODUCTION 1
1.1 Objective 1
1.2 Description of the Buffalo River Area
of Concern 2
1.2.1 Watershed Description 2
1.2.2 Status of Remedial Action Plan 5
1.2.3 Sediment Physical/Chemical Character 5
1.2.3.1 Sources of Sediments 5
1.2.3.2 Sediment Pollution 6
1.2.3.3 Sediment Characteristics and Quality 6
2 DEMONSTRATION APPROACH 13
2.1 Technology Selection 13
2.2 Planning Document 16
2.3 Environmental Assessment 17
2.4 Scope of Work/Contract 17
2.5 Sample Location and Excavation 18
2.6 Site Description 19
2.6.1 Site Preparation 19
2.7 Material Handling 23
2.7.1 Transport 23
2.7.2 Screening 23
2.7.3 Storage 25
2.7.4 Addition of Water 25
2.7.5 Feed Operations 25
11
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TABLE OF CONTENTS (Cont'd)
Paragraph Page
2.8 Thermal Desorption 26
2.8.1 System Description 26
2.8.1.1 Material Handling 27
2.8.1.2 Thermal Processor 30
2.8.1.3 Media Heater 31
2.8.1.4 Off-Gas Control 31
2.8.2 Pilot Scale Demonstration 31
2.8.2.1 Sediment A 32
2.8.2.2 Sediment B 34
2.8.2.3 Sediment C 34
2.8.2.4 Sediment D 35
2.9 Residuals Management 35
2.10 Solidification of Solid Residue 36
2.11 Execution and Costs 38
2.12 Monitoring 39
2.12.1 Process Monitoring by Remediation
Technologies, Inc. (RETEC) 39
2.12.2 Air Monitoring 41
2.12.2.1 Air Monitoring by Remediation
Technologies, Inc. (RETEC) 41
2.12.2.2 Air Monitoring by E-Three, Inc. 43
2.12.3 Corps of Engineers Monitoring 43
2.12.3.1 Sampling 43
2.12.3.2 Analytical Protocol 50
3 RESULTS AND DISCUSSION 50
3.1 Corps of Engineers Results 50
3.1.1 Overall Mass Balance 50
3.1.2 Solids Content 51
3.1.3 Metals 56
3.1.4 Polycyclic Aromatic Hydrocarbons (PAHs) 65
111
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TABLE OF CONTENTS (Cont'd)
Paragraph Page
3.1.5 Solvent Extractables (SE) 69
3.1.6 Total Organic Carbon (TOC) 76
3.1.7 Polychlorinated Biphenyls (PCB) 80
3.1.8 Solidification/Stabilization of
Treated Residue 82
3.2 Full Scale Implementation 85
3.2.1 Thermal Desorption Remediation 85
3.2.1.1 Full-Scale Treatment System 85
3.2.1.2 Cost Estimate for Sediment Remediation 89
3.3 Conclusions and Recommendations 90
3.3.1 Conclusions 90
3.3.2 Recommendations/Lessons Learned 93
IV
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TABLE OF CONTENTS (Cont'd)
TABLES
Number Title Page
1 Inorganic Analysis of Surface Sediment
Grab Samples 7
2 Volatile Organics Data on Surface Sediment
Grab Samples 8
3 PAH Data on Surface Sediment Grab Samples 9
4 Pesticide and PCB Data on Surface Sediment
Grab Samples 10
5 Concentrations of Metals in Ten Buffalo
River Sediment Samples 12
6 Concentrations of Polycyclic Aromatic
Hydrocarbons in Ten Buffalo River
Sediment Samples 14
7A Process Parameter Values as Measured
by RETEC, Inc. (English Units) 33
7B Process Parameter Values as Measured
by RETEC, Inc. (SI Units) 33
8 Solidification/Stabilization Mixes 37
9 Cost of Thermal Desorption
Pilot Scale Demonstration 39
10 Results of Vapor Monitoring by RETEC, Inc. 42
11 Summary of Air Sampling and Analytical
Procedures: E-Three/Battelle 44
12A Air Emissions of Polychlorinated Biphenyls
in Micrograms Per Dry Standard Cubic Meter 44
12B Air Emissions of Particulates in Micrograms
Per Dry Standard Cubic Meter 44
12C Air Emissions of Polycyclic Aromatic Hydro-
carbons in Micrograms Per Dry Standard Cubic
Meter 45
12D Air Emissions of Dioxins in Micrograms Per
Dry Standard Cubic Meter 45
12E Air Emissions of Furans in Micrograms Per
Dry Standard Cubic Meter 46
13 Analytical Parameters for Sediment Samples 47
14 Analytical Parameters for Water Samples 48
15 Solids/Liquids Mass Balance 51
16A Percent Total Solids in Sediment 52
16B Percent Total Solids in Condensate 52
17 Percent Volatile Solids in Sediment 53
18 Correlation Coefficients for Volatile
Solids Removal 56
19A Lead in Sediment 58
19B Lead in Condensate (Filtered) 58
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TABLE OF CONTENTS (Cont'd)
TABLES (Cont'd)
Number Title Page
20A Chromium in Sediment 59
2OB Chromium in Condensate (Filtered) 59
21A Copper in Sediment 60
2IB Copper in Condensate (Filtered) 60
22A Mercury in Sediment 61
22B Mercury in Condensate (Filtered) 61
23A Summary of Calculations: Chromium 63
23B Summary of Calculations: Copper 63
23C Summary of Calculations: Lead 64
23D Summary of Calculations: Mercury 64
24A Low Molecular Weight (< 3 Rings)
PAHs in Sediment 67
24B Low Molecular Weight (< 3 Rings)
PAHs in Condensate 67
25A High Molecular Weight (> 3 Rings)
PAHs in Sediment 70
25B High Molecular Weight (> 3 Rings)
PAHs in Condensate 70
26A Summary of Calculations: Low Molecular
Weight PAHs 71
26B Summary of Calculations: High Molecular
Weight PAHs 71
27A Total PAHs in Sediment 73
27B Total PAHs in Condensate 73
28A Solvent Extractables in Sediment 74
28B Solvent Extractables in Condensate 74
29 Summary of Calculations: Solvent
Extractables 77
30A Total Organic Carbon in Sediment 78
3OB Total Organic Carbon in Condensate 78
31 Summary of Calculations: TOC 80
32A Total PCB in Sediment 81
32B Total PCB in Condensate 81
33 Summary of Calculations: PCB in Solids 82
34 Solidification/Stabilization Unconfined
Compressive Strength (UCS) Results 83
35 Results of Residue stabilization 83
36 Sequential Batch Leach Test (SBLT)
for Metals 84
37 Cost Estimate for Remediating 10,000
Cubic Yards of Sediment 91
38 Cost Estimate for Remediating 100,000
Cubic Yards of Sediment 91
VI
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TABLE OF CONTENTS (Cont'd)
FIGURES
Number Title Page
1 Buffalo River Watershed 3
2 Buffalo River Area of Concern 4
3 Buffalo River Master Station Locations
October 1989 11
4 Sediment Quality Survey 15
5 Location of Confined Disposal Area
Number Four 20
6 Location of Pilot Scale Demonstration 21
7 Plan for Demonstration Site 22
8 Sediment Screening Device 24
8A Thermal Desorption Unit and Screw
Processor 28
9 Flow Diagram for Thermal Desorption
Process 29
10 Demonstration Flow Diagram with Corps
of Engineers Sampling Points 49
11 Percent Solids Versus Exit Temperature
of Solids 54
12 Percent Volatile Solids Versus Exit
Temperature of Solids 55
13 Concentration of Low Molecular Weight
PAHs in Sediment Versus Exit Temperature
of Solids 68
14 Concentration of High Molecular Weight
PAHs in Sediment Versus Exit Temperature
of Solids 72
15 Concentration of Solvent Extractables in
Sediment Versus Exit Temperature of Solids 75
16 TOG (mg/g Solids) Versus Exit Temperature
of Solids 79
17 Results of Residue Stabilization: TOC
Analysis of Extracts From Sequential
Batch Leach Test (SBLT) 86
APPENDIX A
Sample Calculations
APPENDIX B
Unreduced Analytical Data
VII
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LIST OF ABBREVIATIONS AND SYMBOLS
amp
AOC
ARCS
BTU/hr
CDF
DSCM
EA
ETWG
FONSI
g
GLNPO
gpm
HMW
IJC
kg/hr
kw
L
Ibs
Ib/hr
Ibs/sq in
LMW
min
mg
ng
ng/g
NYSDEC
PAH
PCB
ppb
ppm
RCRA
RETEC
SBLT
scfm
TCLP
TOC
TSCA
use
ug/g
ug/1
USEPA
um
v
WES
Cr
Cu
°F
Hg
Pb
pH
r
Zn
ABBREVIATIONS
ampere
Area of Concern
Assessment and Remediation of Contaminated Sediments
British Thermal Unit per hour
Confined Disposal Facility
Dry Standard Cubic Meter
Environmental Assessment
Engineering Technology Work Group
Finding of No Significant Impact
Gram
Great Lakes National Program Office
gallons per minute
high molecular weight
International Joint Commission
kilograms per hour
killowatt
liter
pounds
pounds per hour
pounds per square inch
low molecular weight
minute
milligram
nanogram
nanogram per gram
New York State Department of Environmental Conservation
polycyclic aromatic hydrocarbon
polychlorinated biphenyl
parts per billion
parts per million
Resource Conservation and Recovery Act
Remediation Technologies, Inc.
sequential batch leach test
standard cubic feet per minute
Toxicity Characteristic Leaching Procedure
total organic carbon
Toxic Substances Control Act
unconfined compressive strength
microgram per gram
microgram per liter
United States Environmental Protection Agency
microgram
volt
Waterways Experiment Station
SYMBOLS
chromium
copper
degrees Fahrenheit
mercury
nitrogen gas
percent
lead
- log {H+}
correlation coefficient
zinc
viii
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DISCLAIMER
The information in this document has been funded wholly or in part by the U.S. Environmen-
tal Protection Agency (EPA) under Interagency Agreements No. DW96934688-0,
DW96947515-0, DW96947555-0, DW96947581-0, and DW96947595-0, with the U.S. Army
Corps of Engineers. It has been subjected to the Agency's peer and administrative review
and it has been approved for publication as an EPA document. Mention of trade names or
commercial products does not constitute endorsement or recommendation for use.
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PILOT-SCALE DEMONSTRATION OF THERMAL DESORPTION FOR THE
TREATMENT OF BUFFALO RIVER SEDIMENTS
1.0 INTRODUCTION
The 1987 amendments to the Clean Water Act, Section
118(c)(3), authorized the United States Environmental Protection
Agency's (USEPA) Great Lakes National Program Office (GLNPO) to
conduct a 5-year study and demonstration project on the control
and removal of toxic pollutants in the Great Lakes, with emphasis
on the removal of toxic pollutants from bottom sediments (U.S.
Environmental Protection Agency, 1990). The Great Lakes Water
Quality Board of the International Joint Commission (IJC)
identified 43 Areas of Concern (AOC) in the Great Lakes Basin
where one or more of the objectives of the 1978 Great Lakes Water
Quality Agreement and other jurisdictional standards, criteria,
or guidelines are exceeded. GLNPO initiated the Assessment and
Remediation of Contaminated Sediments (ARCS) Program to assess
the nature and extent of bottom sediment contamination at the
selected AOCs, evaluate and demonstrate remedial options, and
provide guidance on the assessment of contaminated sediment
problems and the selection and implementation of necessary
remedial actions in the AOCs and other locations in the Great
Lakes. The Buffalo River AOC, Buffalo, New York, was one area
specified in the Clean Water Act as requiring priority
consideration in locating and conducting on-site demonstration
projects.
Past industrial and municipal discharges to the Buffalo River
have polluted the river and its sediments. As a result, the
river exhibits environmental degradation and impairment of
beneficial uses of water and biota (New York State DEC, 1989). A
pilot-scale demonstration was conducted in Buffalo, New York in
the fall of 1991 to evaluate the ability of a thermal desorption
process to remediate Buffalo River sediments contaminated with
polynuclear aromatic hydrocarbons (PAHs).
1.1 OBJECTIVE
The objective of the Buffalo River pilot scale treatment
technology demonstration was to evaluate thermal desorption as a
treatment technology for sediments from the Buffalo River Area of
Concern. Specific objectives of the pilot-scale demonstration
included determining: the thermal desorption process1
efficiencies in removing organic contaminants from sediments; the
operating parameters that affect the removal efficiencies; the
equipment necessary to achieve those removal efficiencies; the
pretreatment handling and processing requirements of the
sediments; and the characteristics of each of the process
residual streams and the proper method of disposal for each
residual. Another objective of the demonstration was to provide
technology-specific information to be used in the development of
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cost estimates for full scale remediation projects. In addition,
a solidification process was evaluated by mixing treated
sediments from the thermal desorption process with various
proportions of cementitious material. The solidified blocks were
sampled, and analyzed to determine the effectiveness of the
solidification.
1.2 DESCRIPTION OF THE BUFFALO RIVER AREA OF CONCERN
1.2.1 Watershed Description
The watershed of Buffalo River and its tributaries, Cayuga,
Buffalo, and Cazenovia creeks is located in the west central
portion of New York State (Figure 1). The land area is roughly
triangular in shape. Buffalo and Cayuga creeks originate in the
Allegheny Plateau and flow northwest toward Lake Erie. Buffalo
Creek rises near the town of Java and flows northwesterly to its
confluence with Cayuga Creek in the town of West Seneca. The
drainage area of Buffalo Creek is 150 square miles (New York
State DEC, 1989). Cayuga Creek, with a drainage area of 128
square miles, rises near North Java Station and flows westerly
through the northern part of the Buffalo River watershed. The
confluence of Cayuga Creek and Buffalo Creek form the head of the
Buffalo River.
Cazenovia Creek generally flows north from its head waters near
Springville, New York to its confluence with the Buffalo River
within the Buffalo, New York city limits. The drainage area of
Cazenovia Creek is 138 square miles. From Cazenovia Creek, the
Buffalo River flows westerly to its mouth at the eastern end of
Lake Erie. Overall, the Buffalo River is 8.1 miles in length and
its drainage area is approximately 446 square miles.
The Buffalo River and its sediments have been polluted by over 50
years of industrial and municipal discharge and disposal of
waste. Fishing and quality of aquatic life within the Area of
Concern (Figure 2) have been impaired by heavy metals and
polycyclic aromatic hydrocarbons (PAHs) in sediments. Fish and
wildlife habitat have been degraded by alterations to the river
including modifications to the shoreline such as bulkheading.
Levels of metals and cyanides in the sediment prevent open lake
disposal of sediments dredged from the river. Other potential
sources of pollution to the Buffalo River include inactive
hazardous waste sites, combined sewer overflows, and other point
and non-point sources of pollution. While the Buffalo River
sediments are contaminated, they are not considered "toxic" or
"hazardous" based on strict regulatory definitions, and are
therefore not subject to the appropriate regulations of the Toxic
Substances Control Act (TSCA) or the Resource Conservation and
Recovery Act (RCRA).
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LITTLE BUFFALO CREEK
CAZENWIA CREEK
LAK
E R I
BUFFALO RIVER
LJurrMi_u nivtR j—\
AREA OF CONCERN,/ EAST AURORA \
/ "> •
BUFFALO CREEK
1
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
BUFFALO RIVER
WATERSHED
FIGURE 1
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ERIE
BASIN
MARINA
AREA OF CONCERN
TIMES
BEACH
BUFFALO SHIP CANAL
BUFFALO RIVER
OUTER
HARBOR
CAZENWIA CREEK
LAKE
ERIE
SCALE OF MILES
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
BUFFALO RIVER
AREA OF CONCERN
FIGURE 2
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1.2.2 Status of Remedial Action Plan
New York State Department of Environmental Conservation
(NYSDEC) and other Federal, State, and local agencies have and
continue to carry out remediation of environmental problems along
the Buffalo River. NYSDEC completed and issued the Buffalo River
Remedial Action Plan (RAP) in November 1989. The RAP contained
initial agency commitments to implement the remedial action
strategy. To track implementation of the RAP, NYSDEC has issued
annual reports to illustrate the progress on remediation by
listing accomplishments of the past year and describing
commitments for the current year.
To assist NYSDEC in the remediation process, a Remedial Advisory
Committee (RAC) was formed in 1990. The RAC is representative of
concerned groups within the community that have an interest in
the Buffalo River. These groups include government officials,
public interest groups, economic interests, and private citizens.
The following is a brief summary of RAC activities on the Buffalo
River. A flow activated sampling station was established by
NYSDEC to assist in stream water quality monitoring (New York
State Department of Environmental Conservation, 1992). Event
related sampling has been undertaken and will be continued into
1993. Sediment transport modeling is being conducted by the
USEPA under the ARCS program. A dredging demonstration was
conducted in 1992 by the Corps of Engineers to evaluate the
efficiencies of several dredge types. Phase I investigations for
all 36 inactive hazardous waste sites have been completed, while
all but seven Phase II investigations have been completed.
Remedial Investigation/Feasibility Studies (RI/FS) were completed
for three sites in 1991-92, while two additional RI/FS's are
underway. A combined sewer system model has been developed and
verified for the main interceptors of the Buffalo Sewer Authority
collection system. Operational simulations have been undertaken
and cost estimates of alternatives for overflow
reduction/treatment have been developed. A plan to assess fish
and wildlife habitat conditions and improvement potential has
been developed. Habitat assessment field work has been initiated
by NYSDEC and will be completed in 1993.
1.2.3 Sediment Physical/Chemical Character
1.2.3.1 Sources of Sediments—
The major source of sediment in the Buffalo River is in
runoff from the surrounding watershed. Depending on factors such
as river velocities and discharge, channel topography, bank
erosion and wind, much of the sediment originating in runoff is
either deposited in the river channel bottom or is carried to
areas further downstream. A large portion of this sediment
accumulates in the Buffalo River Federal Navigation Channel.
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1.2.3.2 Sediment Pollution—
The Buffalo River watershed is comprised of three major
streams which converge at or along its mainstem: Cayuga,
Buffalo, and Cazenovia creeks. Within the watershed major land
usage is industrial and commercial, with some agricultural usage.
Flows into the Buffalo River watershed originate in part from a
variety of point and non-point source industrial activities in
the watershed, including inactive hazardous waste sites and
combined sewer outflows/municipal waste discharges (New York
State D.E.C., 1989). These sources contribute to the bottom
sediment contamination in the river. Polynuclear aromatic
hydrocarbons and metals are contaminants of particular concern in
Buffalo River sediments.
1.2.3.3 Sediment Characteristics and Quality—
Historic and recent sediment particle size analyses indicate
that bottom sediments within the Buffalo River are comprised of
silts and clays, with some sands. Particle size and chemical
(inorganic and organic) analyses and 96-hour acute toxicity tests
(bioassays) were performed on surface grab samples obtained from
the Buffalo River Federal Navigation Channel in 1989 (Aqua Tech
Environmental Consultants, 1989). Particle size analysis of the
sediment samples indicates they consist primarily of silts and
clays (approximately 65 to 99 percent), with some sands
(approximately 1 to 35 percent). Regarding inorganic sediment
contamination, the results of bulk inorganic analysis performed
under the 1989 program showed that most of the sediments were
contaminated with elevated levels of numerous metals, including
arsenic, barium, copper, iron, manganese, nickel, and zinc (Table
1). The 1989 sediment testing program included analyses for
volatile organics, PAHs and polychlorinated biphenyls (PCBs).
Table 2 summarizes volatile organics data on sediments.
Generally, volatile organics were not detected in sediments with
the exception of low levels of 1,3-Dichlorobenzene and high
levels of toluene on portions of the Buffalo River. PAH levels,
shown in Table 3, ranged from non-detectable to about 2.4
micrograms per gram (ug/g) (benzo(b)fluoranthene). Total PAHs
ranged from 5.44 to 12.15 ug/g. PCB and pesticide data
summarized in Table 4 show non-detectable levels in the
sediments.
The USEPA's Large Lakes Research Station of Grosse lie, Michigan
sampled sediments along the Buffalo River and Buffalo Ship Canal
in 1989, 1990, and 1991 with a 4-inch diameter vibracore unit.
Results from testing performed on samples collected outside the
navigation channel in 1989 show concentration levels for 12
metals at 10 sites along the Buffalo River (Figure 3 and Table
5). Concentration levels for chromium (Cr) ranged from less than
13 ug/g to 312 ug/g while concentration levels for mercury (Hg)
ranged from 0.0109 to 1.93 ug/g. Lead (Pb) concentrations ranged
from 28 to 314 ug/g while zinc (Zn) concentrations ranged from 32
to 900 ug/g. In general, the highest concentration levels of
metals were in the terminal end of the Buffalo Ship Canal and in
the middle third reach of the Buffalo River. Test results
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TABLE 1
INORGANIC ANALYSIS OF SURFACE SEDIMENT GRAB SAMPLES
ug/g (dry)
Bulk inorganic analysis of surface sediment grab
samples collected from Buffalo River, Erie County,
New York. Sediment sampling areas are shown in
Figure 4.
Sediment Sampling Areas
Inorganic
Parameter
ARSENIC, TOTAL, AS
BARIUM, TOTAL, BA
CADMIUM, TOTAL, CD
CHROMIUM, TOTAL, CR
COPPER, TOTAL, CU
IRON, TOTAL, FE
LEAD, TOTAL PB
MANGANESE, TOTAL, MN
MERCURY, TOTAL, HG
NICKEL, TOTAL, NI
RESIDUE, TOTAL (TS), %
SELENIUM, TOTAL, SE
SILVER, TOTAL, AG
SODIUM, TOTAL, HA
SPECIFIC GRAVITY
CARBON, TOTAL ORGANIC, C
ZINC, TOTAL, ZN
Deadman1
13
90
0.5
18
49
30300
82
490
0.40
31
48.7
<1
<0.5
440
1.41
1400
210
s Creek
11
84
1
13
46
29200
66
490
0.37
30
53.4
<2
<0.5
450
1.5
1200
210
Hamburg Street
10
79
1
13
48
28400
62
460
0.34
29
55.2
<2
<0.6
440
1.48
1000
180
Blue Tower
Turning Basin
9
91
0.6
9
40
30800
55
480
0.28
32
50.6
<2
<0.6
500
1.48
1200
170
Mobi I
10
78
1
2
35
24300
60
520
0.24
25
57.0
<2
<0.6
430
1.56
1100
120
Oil
7
81
<0.6
4
35
20500
25
530
0.06
22
40.3
<2
<0.6
360
1.22
2200
940
DATA SOURCE: Referenced Aqua Tech Report
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-------
TABLE 3
PAH DATA FOR SURFACE SEDIMENT GRAB SAMPLES
ug/g (dry)
PAH data on surface sediment grab samples collected
from Buffalo River, Erie County, New York. Sediment
sampling areas are shown in Figure 4.
Sediment Sampling Areas
PAH
Acenaphthene
Acenaphthylene
Anthracene
Benzo(a) Anthracene
Benzo(a)Pyrene
Benzo(b)Fluoranthene
BenzoCghi )Perylene
Benzo(k)Fluoranthene
Chrysene
Dibenzo(a,h)Anthracene
Fluoranthene
Fluorene
Indeno(1,2,3-cd)Pyrene
Naphthalene
Phenanthrene
Pyrene
Total PAHs
Deadman's
<0.20
<0.20
0.13
0.58
0.79
1.58
<0.40
<0.20
0.73
<0.40
1.36
<0.30
0.44
<0.30
0.58
0.83
7.02
Creek
<0.20
<0.20
0.34
0.93
1.37
2.38
0.49
<0.20
0.98
<0.40
2.33
<0.30
0.61
<0.30
1.34
1.38
12.15
Hamburg Street
<0.20
<0.20
0.16
0.51
0.81
1.45
<0.40
<0.20
0.57
<0.40
1.30
<0.30
0.41
<0.30
0.59
0.72
6.52
Blue Tower
Turning Basin
<0.20
<0.20
0.13
0.45
0.86
1.49
<0.40
<0.20
0.63
<0.40
1.21
<0.30
<0.30
<0.30
0.59
0.76
6.12
Mobi I
<0.20
<0.20
0.14
0.46
0.74
1.21
<0.40
<0.20
0.52
<0.40
1.05
<0.30
<0.30
<0.30
0.60
0.83
5.55
Oil
<0.20
<0.20
0.12
0.39
0.68
1.11
<0.40
<0.20
0.43
<0.40
1.21
<0.30
<0.30
<0.30
0.78
0.72
5.44
DATA SOURCE: Referenced Aqua Tech Report
-------
TABLE 4
PESTICIDE AND PCB DATA FOR SURFACE SEDIMENT GRAB SAMPLES
ug/g (dry)
Pesticide and PCB data on surface sediment grab samples
collected from Buffalo River, Erie County, New York.
Sediment sampling areas are shown in Figure 4.
Sediment Sampling Areas
Pesticides and
PCB
Aldrin
alpha-BHC
beta-BHC
gamma-BHC
delta-BHC
Chlordane
4,4'-DDD
4,4'-DDE
4,4'-DDT
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan Sulfate
Endrin
Endrin Aldehyde
Heptachlor
Heptachlor Epoxide
Toxaphene
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB -1248
PCB- 1254
PCB- 1260
Deadman1
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
<0.05
<0.03
<0.03
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
's Creek
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
<0.05
<0.03
<0.03
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
Hamburg Street
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
0.06
<0.03
<0.03
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
Blue Tower
Turning Basin
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
<0.05
<0.03
<0.03
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
Mobi I
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
<0.05
<0.03
<0.03
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
<0.10
Oil
<0.02
<0.02
<0.02
<0.02
<0.02
<0.10
<0.02
<0.03
<0.03
<0.02
<0.03
<0.03
<0.03
<0.05
<0.05
<0.03
0.05
<0.10
<0.10
<0.10
<0.10
<0.10
O.10
<0.10
<0.10
DATA SOURCE: Referenced Aqua Tech Report
10
-------
CANAL
UPSTREAM
OUTER
HARBOR
CAZENOVIA
BUFFALO RIVER
LAKE
ERIE
SCALE OF MILES
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
07011 - USEPA MASTER/
INDICATOR STATION
BUFFALO RIVER
MASTER STATION LOCATIONS
OCTOBER 1989
FIGURE 3
11
-------
TABLE 5
CONCENTRATIONS OF METALS IN TEN BUFFALO RIVER
SEDIMENT SAMPLES (OCTOBER, 1989)
ug/g (dry) (except % Fe)
SAMPLING LOCATIONS ARE SHOWN IN FIGURE 3
Sample
0101
0201
0301
0401
0501
0601, Rep 1 (a)
0601, Rep 2 (a)
0701
0801
0901
1001
A?
0.46
<0.03
0.44
0.22
0.16
0.21
0.24
0.13
0.13
0.12
0.12
As cd Cr
34
<1.4
13
12
<4.5
13
12
12
12
11
8.2
4.0
0.035
1.4
1.0
1.6
1.2
1.2
0.90
0.70
0.69
0.57
312
<13
113
77
100
110
130
92
70
56
46
Cu
148
8.2
67
50
60
90
93
49
46
41
35
%Fe
5.5
0.33
4.4
4.2
5.4
4.2
4.2
4.1
3.7
3.4
3.0
Hg
1.93
0.019
0.624
0.186
0.329
1.62
1.76
0.233
0.132
0.066
0.082
Mn
1,386
40
685
790
673
630
630
730
730
730
560
Hl_
57
5.2
45
50
47
52
46
44
43
40
34
Pb
286
28
107
67
314
140
150
70
51
49
43
Se Zfi
3.8
<0.49
<0.92
<0.85
<1.0
0.93
<0.89
<0.86
<0.88
<0.84
<0.83
900
32
286
220
371
390
390
200
170
160
140
(a) Duplicate Samples Collected at Buffalo River Station 0601
DATA SOURCE: Environmental Protection Agency (Unpublished)
12
-------
for 20 organic parameters (PAHs) analyzed at 9 of the 10 sampling
sites are given in Table 6. Generally the highest concentration
of PAHs were at sample site 0601 in the Buffalo River and 0101 at
the terminal end of the Buffalo Ship Canal. Benzo(a)pyrene
concentrations ranged from undetectable at 54 nanogram per gram
(ng/g) to 2500 (ng/g) at sample site 0601.
In 1990 and 1991 sediment vibracore samples were collected by
USEPA in the Buffalo River. Generally, approximately 1 to 3
meter core samples were taken and analyzed. Analytical results
indicated that sediment contamination is either (1) relatively
low and consistent with respect to depth, or (2) increases with
respect to depth to a maximum level at which point a relatively
clean, natural lacustrine clay layer is reached (U.S. Army
Engineer District, Buffalo, 1992).
Areas sampled during the 1991 program are shown on Figure 4.
Results of the 1991 sampling revealed that, in general, lightly
to moderately polluted sediments overlay heavily polluted
sediments as shown in concentrations of chromium, lead, zinc, and
PAHs. Some of the core samples extended through the heavily
polluted sediments into underlying moderately and lightly
polluted sediments at core depths of roughly 3 to 4 meters. Many
of the vibracore samples met refusal at a depth of 3 meters or
less and did not appear to penetrate deep enough to extend
through the heavily polluted sediments and into the underlying
moderately and lightly polluted sediments.
2.0 DEMONSTRATION APPROACH
2.1 TECHNOLOGY SELECTION
A literature review of treatment technologies was performed
for the ARCS Program by the Corps of Engineers Waterways
Experiment Station (WES) and was used to screen process options
for biological, chemical, extraction, immobilization, radiant
energy, and thermal technologies (Averett, 1990b). Each process
option was assessed on the basis of effectiveness,
implementability, and cost. A number of the higher cost thermal
processes were eliminated from consideration due to the expense
of these processes while numerous other processes were eliminated
from further consideration because of the lack of research and
development for application to a specific sediment and associated
contaminant matrix. The availability of a mobile pilot scale
unit was essential for implementing an on-site pilot
demonstration. Based on these criteria, a list of those
processes that should be retained for demonstration consideration
was developed.
A matrix was developed for the processes recommended for
consideration for the pilot scale demonstrations, the principal
contaminants treatable by each process, and the Areas of Concern
13
-------
TABLE 6
CONCENTRATIONS OF POLYCYCLIC AROMATIC HYDROCARBONS
IN TEN BUFFALO RIVER SEDIMENT SAMPLES (ng/g)
SAMPLING LOCATIONS ARE SHOWN IN FIGURE 3
Compound
0101 0201 0301 0401 0501 0601
0701
0801 0901 1001
Polvcvclic Aromatic Hydrocarbons:
Naphthalene
2-methylnaphthalene
Acenaphthylene
Acenapthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-c,d)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
8600 U57(a) 360 U35
1000 U57 180 U35
670 U61 U50 U37
300 U61 U50 U37
770 U61 310 U37
2600 U71 1100 300
720 U68 810 88
3200 U110 1400 620
2600 U140 1600 460
1500 U43 520 240
1700 U54 810 320
3000 U61 770 330
4000 U82 690 340
2500 U54 360 320
1600 U89 400 U54
350 U68 U56 U41
1600 U110 470 U67
140 830 150
150 2200 U42
U45 U45 U45
U45 750 U45
300 3600 160
2100 11000 750
500 4500 260
2100 5400 1100
1900 7100 1200
690 1900 520
980 2700 770
1100 1600 740
970 1600 660
930 1300 690
500 1000 270
U50 U50 U50
370 1100 290
U38 U30
U38 U30
U40 U31
U40 U31
U40 U31
370 380
96 U35
610 840
560 530
210 220
360 330
440 430
300 320
280 310
U60 160
U45 U35
U74 170
(b)
(a) - U57 Indicates a Sample Concentration Below the Detection Limit of 57 PPB
(b) - Data Not Yet Available
DATA SOURCE: Environmental Protection Agency (Unpublished)
14
-------
ERIE
BASIN
MARINA
1991 SEDIMENT SAMPLING AREA
TIMES
BEACH
BUFFALO SHIP CANAL
DRY DOCK COVE
DEADMAN'S CREEK
HAMBURG STREET
BUFFALO RIVER
MOBIL OIL
OUTER
ARBOR
BLUE TOWER TURNING BASIN
LAKE
ERIE
SCALE OF MILES
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
^ BUFFALO RIVER SEDIMENTS
SEDIMENT QUALITY
SURVEY
FIGURE 4
-------
where such contaminants are present and the processes are
applicable (Averett, 1990a). A list of potential pilot projects
was then prepared and these alternatives were ranked for
consideration based on factors affecting their selection.
All five priority sites, Ashtabula River, Ohio; Buffalo River,
New York; Grand Calumet River, Indiana; Saginaw River, Michigan;
and Sheboygan Harbor, Wisconsin are contaminated by organic
compounds. Most of these sites have areas of elevated
contamination that could be used for a demonstration project.
Rather than strictly following the numeric ranking of the
potential pilot scale demonstrations, the ARCS
Engineering/Technology Work Group (ETWG), responsible for
recommending and implementing the demonstration, determined that
a variety of the technology groups (biological, chemical,
extraction, immobilization, thermal) should be selected for
demonstration. With this in mind, thermal desorption, a
technology suitable for treating materials contaminated with
organics, was selected for a pilot scale demonstration to be
conducted at the Buffalo River Area of Concern.
2.2 PLANNING DOCUMENT
Buffalo District initiated its planning for the pilot-scale
demonstration in the fall of 1990. Coordination efforts
associated with the demonstration involved meetings,
correspondence, and telephone conversations with representatives
of USEPA Region II, NYSDEC, members of the Buffalo River Remedial
Action Committee, as well as the Corps of Engineers Regulatory
personnel. A meeting was held with NYSDEC personnel in September
1990, while the October 1990 meeting of the ARCS ETWG was held at
the NYSDEC Region 9 headquarters in Buffalo, New York. Topics
discussed in these meetings included the thermal desorption
technology, the scope and proposed location of the demonstration,
anticipated treatment process residuals and their disposal and
regulatory requirements. A document entitled" Work Plan for
Pilot-Scale Demonstration for Remediation of Contaminated
Sediments at the Buffalo River Area of Concern," was completed in
February 1991. This report addressed sediment quality,
description of the Buffalo River AOC, selection of the treatment
technology, description of the demonstration, ranging from
sediment removal and transport to residuals management and an
estimate of all costs associated with the project. Also included
was a description of activities associated with the demonstration
ranging from regulatory and contractual requirements to
monitoring requirements and report preparation. Members of the
ETWG, including USEPA Region II, State and local representatives,
were given the opportunity to review and comment on the document.
Comments were reflected in the final document which was approved
by the ETWG.
16
-------
2.3 ENVIRONMENTAL ASSESSMENT
In early 1991, the Corps of Engineers Buffalo District
initiated work on an Environmental Assessment (EA). The
assessment provided background information and addressed the
environmental impacts and statutory compliance of the project.
Social impacts were discussed as were the effects of the project
on natural resources including air and water quality, aquatic and
terrestrial habitat, and threatened and endangered species. A
brief description of the various environmental regulations and
statutes applicable to the demonstration project and the degree
to which the project was in compliance with those statutes and
regulations was provided. Since no new dredged materials were to
be discharged below Low Water Datum and given the small scope of
the project, it was determined that the dredging of the sediments
to be remediated fell within the limits specified under Section
10 of the Clean Water Act (Nationwide Permit No. 19) and complied
with the provisions of Section 404(b) of the Clean Water Act. A
404(b)(l) Evaluation was not necessary since the discharge of
dredged material from the Buffalo Harbor into confined disposal
facility No. 4 is covered under the 404(b)(l) Evaluation and
Water Quality Certificate prepared for the construction of the
disposal facility and any subsequent dredging connected with the
facility. The project was also found to be in compliance with
the River and Harbor Act of 1970, the Endangered Species Act of
1973, as amended, and numerous other applicable acts. With the
dissemination and distribution of the EA and its associated
Finding of No Significant Impact (FONSI) to numerous Federal,
State, and local agencies and individuals, the project was found
to be in full compliance with the National Environmental Policy
Act. The FONSI was completed and signed on August 19, 1991.
2.4 SCOPE OF WORK/CONTRACT
A scope of work was prepared for a pilot scale demonstration
of the remediation of contaminated sediments at the Buffalo River
Area of Concern utilizing thermal desorption. This scope of work
provided background information, stated the objective of the
demonstration, and provided a detailed description of the
services required. The scope of work was made a part of the
request for proposals that was provided to 36 interested firms
responding to an announcement published in the Commerce Business
Daily. The two proposals submitted in response to the request
for proposals were reviewed by members of the ETWG to determine
the prospective firms abilities to conduct the required services.
The technical proposals were evaluated using a rating system
based on the technical evaluation criteria developed by the ETWG
and presented in the Commerce Business Daily announcement.
Contract award was based on a firm's ability to meet the
technical requirements of the testing involved, the company's
qualifications and experience in conducting similar studies, the
uniqueness and innovativeness of the technology in treating Great
Lakes sediments, a comparison of cost estimates,
-------
and the feasibility of conducting a full scale remediation
project with the contractor's technology. After this evaluation
was performed, a contract was awarded to Remediation
Technologies, Inc. (RETEC) of Concord, Massachusetts.
2.5 SAMPLE LOCATION AND EXCAVATION
Based on available sediment sampling and analysis data
obtained by the USEPA from 1989 and 1990 sampling operations,
there were two areas of the Buffalo River Area of Concern where
the sediments generally had higher concentrations of PAHs, than
remaining portions of the river. These two areas were near the
terminal end of the Buffalo Ship Canal and in an area of the
upper portion of the Buffalo River Federal Navigation Channel.
The contaminated sediments for the pilot scale demonstration came
from the Buffalo River since this area had been sampled and
tested in much more detail than the Buffalo Ship Canal, and,
therefore it was anticipated that a sediment sample could be
located and collected with greater assurance that it would
contain significant concentrations of PAHs. It was desirable to
treat more highly contaminated sediments during this
demonstration since these are the sediments that are likely to be
treated during any full scale remediation.
Sediments collected from the Buffalo River were used to evaluate
the treatment technology rather than using sediments already
deposited in the Corps of Engineers Confined Disposal Facility
(CDF) No. 4 in Buffalo Harbor. Some of the PAHs contaminating
the Buffalo River sediments are volatile and may escape the
sediments when exposed to the atmosphere for significant lengths
of time, or when they are rehandled several times, as sediments
from the CDF would have been. Therefore, fresh sediments were
collected for the pilot demonstration to ensure that significant
amounts of the PAH contaminants did not volatilize prior to
treatment.
The excavation of the contaminated sediments from the Buffalo
River was accomplished by using floating plant consisting of a
barge mounted crane and tug boat owned by Manson Construction Co.
Inc. and under contract to the Corps of Engineers. An open
clamshell bucket dredged approximately 15 cubic yards of
sediments to be treated in the thermal desorption unit. Four to
six feet of sediment was excavated in 10 to 12 feet of water at
USEPA sample point 2501 and placed in four waste disposal bins
(dumpsters) labeled "A" through "D" on the barge deck.
Preliminary analytical results indicated that sediments at this
location contained elevated levels of extractable residues from
the surface of the sediments to 6 to 8 feet below the surface of
the sediments.
18
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2.6 SITE DESCRIPTION
While other sites along the Buffalo River were considered,
the demonstration was conducted within the confines of Buffalo
District's CDF No. 4 due to several advantages of this site over
privately owned or public lands that may have been available
within the Area of Concern. Issues of liability and access were
greatly simplified since the facility is owned by the Corps of
Engineers. In addition, regulatory requirements had already been
satisfied for using this facility to confine contaminated dredged
sediments. The CDF had been designed and constructed in the mid
1970s to contain polluted sediments dredged from the Buffalo
River and Buffalo Harbor. Community concerns would be eased if
the demonstration were conducted within CDF No. 4 since it is
located in an area removed from any housing or public access.
Finally, the remoteness of the area minimized security problems.
Excavated sediments were transported by barge to CDF No. 4
(Figure 5). Contamination of the surrounding water bodies due to
spillage was controlled by avoiding overloading the waste bins
with sediment material. Transfer of the bins from the barge to
the CDF was accomplished through the use of the barge mounted
crane. The floating plant was secured in Buffalo Harbor,
adjacent to the CDF, while the waste bins containing the dredged
sediments were off-loaded onto Stoney Point Breakwater, the
eastern boundary of the disposal facility (Figure 6).
CDF No. 4 is located at the southern end of the Buffalo Harbor,
adjacent to the Bethlehem Steel Corporation's Lackawanna plant.
Access to the CDF is available though the Bethlehem Steel plant.
The pilot scale demonstration took place along the east side of
the disposal facility, adjacent to the Stoney Point Breakwater
(Figure 6). An existing access road along this portion of the
dike was capable of carrying vehicular traffic, including tractor
trailers loaded with demonstration equipment. Several acres were
available within the disposal facility upon which the
demonstration could be conducted. This included an area of 2 to
3 acres adjacent to the roughly 300-foot long pumpout pipe. This
area was generally clear of trees and shrubs and was relatively
level,' though it did contain approximately 1 to 3 foot
undulations in the surface contours.
2.6.1 Site Preparation
Prior to their mobile pilot scale unit arriving on site,
Remediation Technologies, Inc. (RETEC) prepared the site. An
area of roughly 10,000 square feet was cleared and prepared for
the mobile thermal processor and support equipment which
included: chiller, electric generator, water tank, inert gas
tank (Nitrogen gas), office trailer, storage trailer, publicity
tent, and drum storage area (Figure 7). Sufficient area was also
available to provide parking for several vehicles. The
demonstration area was constructed using a bulldozer to remove
the surficial soils and stockpile them along
19
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CORPS OF ENGINEERS
DISPOSAL AREA
NUMBER 4
PILOT
DEMONSTRATION SITE
CITY
OF
BUFFALO
LAKE
ERIE
LACKAWANNA CANAL
USEPA SAMPLE POINT 2501
SCALE OF MILES
'/„
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°'4
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
LOCATION OF
CONFINED DISPOSAL AREA
NUMBER 4
FIGURE 5
20
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EXISTING LIGHTHOUSE
BUFFALO HARBOR
FIXED PLATFORM
PILOT DEMONSTRATION SITE
EXISTING STONEY POINT
BREAKWATER
CONFINED
DISPOSAL FACILITY
NUMBER 4
SCALE: 1" = 400'
0 /ion'
PILOT-SCALE DEMONSTRATION
Z" THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVFR SEDIMENT^
LOCATION OF
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PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
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PLAN FOR
DEMONSTRATION SITE
FIGURE 7
-------
the western edge of the site. Approximately 300 tons of slag was
applied to the cleared area to provide a firm working surface and
improve water drainage. The slag material, purchased by
Remediation Technologies, Inc. from the adjacent Bethlehem Steel
plant, was spread with a bulldozer and compacted with a vibratory
roller. RETEC performed site preparation and mobilized the pilot
scale thermal desorption processor and support equipment to the
site from October 7 through October 18, 1991.
2.7 MATERIAL HANDLING
2.7.1 Transport
The dredged sediments were placed into four dumpsters aboard
the floating plant and transported to CDF No. 4 by Manson
Construction Co. on October 7, 1991. Approximately 4 cubic yards
of sediments were placed in each of four bins labeled "A" through
"D" in order to track the sediments during the treatability
study. Transfer of the dumpsters from the deck of the floating
plant to CDF No. 4 was accomplished through the use of Hanson's
barge mounted crane. At this point, the sediments were turned
over to the remediation contractor, RETEC, for pretreatment and
treatment operations.
2.7.2 Screening
Prior to pilot scale treatment of the excavated sediment
using the thermal desorption technology, it was necessary to
remove particles and debris greater than 0.75 inches in size from
the feed sediments. RETEC fabricated a sediment screening device
which provided the capability of simultaneously filling four 55-
gallon drums (Figure 8). The device covered an area 16 square
feet in size and had four holes cut into it, each the size of a
55-gallon drum. An inflexible wire mesh was welded to each hole
to screen objects greater than 0.75 inches in size. The
screening device had 1 foot high walls and was capable of holding
several cubic feet of material, the equivalent of a small backhoe
bucket.
A backhoe was used to remove approximately 12 cubic yards of the
sediments from the four dumpsters and place it in the screening
device. Three cubic yards of sediment that could not be removed
by backhoe were later removed by hand and disposed of in the CDF.
The screening device was designed to allow undersized material to
pass the wire mesh and fall into the 55-gallon drums by gravity.
However, the cohesive nature of the sediments dredged from the
Buffalo River for this demonstration prevented the material from
passing through the screen by gravity. RETEC personnel then
tried to use shovels to force the sediments through the screen
with little success. They then used a backhoe bucket to force
the sediments through the screen. This approach turned out to be
time consuming and extremely inefficient. Screening by hand was
the most efficient means found to screen the oversized material
23
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-------
from the sediments during the demonstration project. Each
backhoe bucket full of sediments was handled by RETEC personnel
outfitted in protective tyvek suits and gloves. Oversized
material screened from the sediments consisted mostly of gravel
and tree branches and amounted to well under 1 percent (by weight
and volume) of the screened sediments. Oversized material was
disposed of within the confined disposal facility while the
screened material was stored in covered 55-gallon drums prior to
being treated using the RETEC thermal desorption process.
2.7.3 Storage
The 12 cubic yards of screened sediments were stored in 48
covered 55-gallon drums from the time they were screened, October
8 and 9, until the sediment was treated in the thermal desorption
unit, between October 21 and November 25, 1991. Approximately 3
cubic yards of sediment were screened from each of the four bins
(labeled A thru D) into twelve 55-gallon drums. The twelve drums
from each bin of sediment were split into three groups of four
drums each and labeled Al (four drums), A2, A3, Bl, B2, B3, Cl,
C2, C3, Dl, D2, and D3.
2.7.4 Addition of Water
Just prior to feeding the sediments for a particular run
into the thermal unit, RETEC personnel mixed water with the four
drums of sediment to be treated. The water content of the
dredged sediments was relatively consistent, ranging from 40 to
45 percent. A relatively small amount of water, 2 to 3 percent,
was added to the sediments from bin "A" in order to assist the
feed operations by increasing the "pumpability" of the feed
material. The water was added to each 55-gallon drum of sediment
while the sediments were being mixed with an electric powered
paddle mixer. The water content of the sediments from bins "B,"
"C," and "D" were similarly adjusted to approximately 45, 50, and
60 percent, respectively.
2.7.5 Feed Operations
The normal material handling system for the thermal
desorption unit was a bucket conveyor designed for bulk solid
material, which appeared ineffective for feeding the high
moisture, cohesive sediments dredged for the pilot scale
demonstration. The contractor, RETEC, based this judgment on a
simple field test, whether or not the sediments stuck to a spoon
when the spoon was inverted. The Buffalo River sediments
remained stuck to the spoon and, therefore, feeding the material
into the thermal unit with the bucket conveyor was not attempted.
For this demonstration, the sediments were fed into the processor
by means of a diesel-powered peristaltic pump. The peristaltic
pump was designed to provide a continuous and steady delivery of
material to the thermal unit. The manufacturer described the
pump as capable of processing up to 80 percent solids and
particle sizes up to 0.75 inches in size. It was rated to have a
25
-------
maximum delivery rate of 110 gallons per minute at a suction head
of 29 feet. Initial project delays were encountered while
waiting for site delivery of the pump from the manufacturer and
in defining the proper material of construction for the
peristaltic hose. A natural rubber material was finally selected
on the basis of its resiliency. RETEC found the pump
unsuccessful in pumping the screened sediments until a small
amount of water was added as described above. Sediments were
pumped into the thermal system just below the slide gate (air
lock) on the processor to minimize infiltration of ambient air
into the processing chamber.
2.8 THERMAL DESORPTION
Thermal desorption refers to the separation of contaminants
from a solid matrix by heating to volatilize organic
contaminants. The desorption process can be used in conjunction
with separate processes, such as incineration, condensation, or
adsorption, for subsequent control of the volatilized
constituents. According to Remediation Technologies, Inc. the
fact that, for some contaminants, efficient removals can be
achieved at relatively low treatment temperatures makes thermal
desorption a less costly approach than incineration for the
remediation of solids contaminated with organic constituents.
The desorption process is not effective in treating materials
contaminated with inorganic contaminants.
The desorption process can be accomplished using various types of
direct or indirect fired equipment. Applications using
indirectly-fired methods are preferred in many cases since they
generate a significantly smaller volume of off-gas than
traditional drying or incineration systems. As a result, the
capital and operating costs for the system can be significantly
reduced.
2.8.1 System Description
Remediation Technologies, Inc. has developed a thermal
desorption technology that reportedly has demonstrated
applications as both a pre-treatment operation (dewatering,
removal of volatile constituents) and final treatment operations
for waste water treatment sludges from petroleum refineries as
well as soils contaminated with organics (Remediation
Technologies, Inc., 1992). RETEC's application of the technology
relies on condensation to capture most of the organics
volatilized by the thermal processor. Volatilized organics are
condensed into a concentrated liquid stream which can
subsequently be managed either on-site using further treatment
systems or off-site at a permitted treatment/storage/disposal
facility. The benefits of the system include lower capital costs
relative to traditional thermal technologies, and permitting
requirements that are less stringent than for incineration
systems.
26
-------
RETEC's system is based upon the use of an established,
indirectly-heated thermal desorption/dryer system, the Holo-Flite
Screw Processor, manufactured by the Denver Equipment Company,
Colorado Springs, Colorado. The Holo-Flite processor is an
indirect-heat exchanger commonly used to heat, cool, and dry bulk
solids and slurries. The treatment system consists of a jacketed
trough which houses a heated double-screw mechanism. The
rotation of the screws promotes the forward movement of the
material through the processor. The rotating augers are arranged
in the trough so that the flights of the two screws mesh,
facilitating the movement of material and improving the heat
transfer.
The RETEC processor uses a contained, non-contact circulating
heat transfer media to elevate the temperature of the solids.
The heated media continuously circulates through the hollow
flights of the screw augers, travels the full length of the
screws, and returns through the center of each shaft to the
heater. The heat transfer fluid is also circulated through the
trough jacket to provide additional heat transfer surfaces for
improved volatilization. RETEC's system employs a unique heat
transfer medium, a molten salt eutectic consisting of 53 percent
potassium nitrate, 40 percent sodium nitrite, and 7 percent
sodium nitrate. The use of this media provides the ability to
achieve processing temperatures up to 850°F to effect appropriate
removals of heavier organic species and increase the efficiency
of the system in treating more complex solid matrices. In
addition to the enhanced thermal properties, the salt eutectic
provides significant safety benefits; the salt melt is non-
combustible, it provides no risk of explosion, and potential
vapors are non-toxic (Remediation Technologies, Inc., 1992). An
inert atmosphere was maintained in the thermal treatment chamber
through the controlled introduction of nitrogen gas to ensure
that oxidation of the volatilized material did not occur.
Remediation Technologies, Inc. utilized its transportable
demonstration system for the performance of this project (Figure
8A). The system, contained on a single 8-foot by 45-foot flat
bed trailer, consisted of material feed equipment, thermal
processor, indirect condensing system, and an activated carbon
unit for the control of volatile organic constituents. A process
flow diagram for this pilot scale system is shown in Figure 9.
The design of the demonstration unit utilizes manual general
control systems that are not equipped with feed interlocks.
2.8.1.1 Material Handling—
Generally, material to be processed by RETEC in their
thermal desorption system is placed in a live bottom feed storage
hopper with a 1.5 cubic yard capacity. The material is sized and
conveyed to a bucket elevator using twin 6-inch diameter screws
equipped with ribbon flights. The bucket elevator raises the
material to a height of 17 feet to a feed auger which uses a
single 6-inch ribbon flight screw to convey the material to the
processor via a double slide gate (air lock). The slide gate is
to prevent the leakage of ambient air into the processor.
27
-------
Figure 8A: Thermal desorption unit and screw processor
Thermal desorption unit at Buffalo River pilot demonstration site
Holo-flite screw processor
28
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AQUEOUS
CONDENSATE
CONTINUOUS MONITORING 02
PUMP
SOLIDS
TO ATMOSPHERE
I
CONTINUOUS MONITORING —
STACK
RETEC GAS SAMPLE LOCATION —(G)
RETEC SOLID SAMPLE LOCATION —(?)
RETEC LIQUID SAMPLE LOCATION —Q
L1A AND L1B WERE COMBINED TO
FORM AQUEOUS CONDENSATE
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
FLOW DIAGRAM FOR THERMAL
DESORPTION PROCESS
FIGURE 9
29
-------
As stated previously, due to the cohesive nature of the Buffalo
River sediments, a diesel powered peristaltic pump was used to
deliver the screened Buffalo River sediments to the thermal
processor during this demonstration project. The pump consisted
of a 5 horsepower air cooled diesel engine attached to a high
capacity peristaltic pump head. The flow rate of the pump was
rated at 110 gallons per minute maximum. During this
demonstration, the sediments were drawn through the pump at an
average feed rate of I gallon per minute. A 2-inch diameter hose
was used to draw the feed material from the 55 gallon drums and
deliver them to the thermal processor. The pump discharge line
was connected to the processor after the double slide gates (air
lock).
2.8.1.2 Thermal Processor—
The Holo-Flite thermal processor contained two 7-inch
intermeshing screw conveyors and had the nominal capacity to
treat 0.5 tons per hour of material (Figure 8A). The system was
operated at media temperatures and solids residence times that
allowed the solids to achieve temperatures in the range of 300 to
540°F. At these temperatures, organic constituents and moisture
present in the waste material were volatilized and drawn away
under negative pressure to the off-gas control system. Solids
residence times in the processor were varied from 30 to 90
minutes through the use of a variable speed drive for the
rotating augers.
The atmosphere in the treatment chamber was controlled during all
treatment activities. The pressure inside the processor was
maintained at -0.1 to -0.5 inches of water column and an "inert"
atmosphere was maintained in the treatment chamber through the
controlled introduction of nitrogen. RETEC used a commercially
provided tank as the source of inert gas. The nitrogen (N2) gas
was delivered to the processor at a flow rate of 5 to 30 cubic
feet per minute. The oxygen content of the gas stream was
monitored continuously during the operation of the treatment
system to ensure that oxidation of the volatilized materials
would not occur. Oxygen levels were consistently maintained
below 17.5 percent.
Treated solids were fed by gravity to a second process auger
designed to cool the solids prior to exiting the desorption unit.
The "cooling screw" was also of the Holo-Flite design and used a
single auger with chilled water as the cooling media. The
cooling screw reguired approximately 12 gallons per minute (gpm)
of water less than 90°F to cool the treated solids to a
temperature of approximately 140°F. The temperature of the water
was maintained using a closed-loop chiller system. The treated
solids were discharged from the cooler through a rotary air lock
into 55-gallon drums.
30
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2.8.1.3 Media Heater—
The salt eutectic was stored and heated in an enclosed,
insulated stainless steel vessel having a capacity of
approximately 600 gallons. The eutectic was heated electrically
using 27 immersion heaters capable of providing one million BTU
per hour of heating capacity to the unit and media temperatures
of approximately 1,000°F. The heat medium was delivered to the
thermal processor by means of a vertical pump with a submersible
head. The pump had the capability to deliver up to 50 gpm of
molten salt eutectic to the processor.
2.8.1.4 Off-Gas Control—
The off-gas control system was designed to accommodate an
off-gas flow rate of approximately 150 standard cubic feet per
minute (scfm) and a "worst case" moisture and organic loading of
400 pounds per hour and 150 pounds per hour, respectively. Two
particulate cyclones were used to remove any fine solid particles
(greater than 10 microns) which may have been entrained with the
off-gases. These solids were removed on a daily basis and
combined with the treated solids for subsequent disposal. Two
indirect heat exchangers, having a combined surface area of 200
square feet, were used to reduce the temperature of the gas
leaving the processor to approximately 120°F and condense the
majority of the entrained moisture and organics. An after
cooler, condenser number 3, was placed in line to remove the
remaining moisture and volatile organics from the off-gas stream
(Figure 8). The exchanger was designed to achieve an exit gas
temperature of 50°F. Cooling water was recirculated in a closed
loop through a chiller having a capacity of 240,000 BTU per hour.
Condensates were collected in two separate vessels prior to
transfer from the system. The system was driven by a variable
speed rotary blower capable of developing 300 scfm of flow at a
vacuum of 3 inches of mercury.
The thermal system was equipped with an activated carbon system
to control noncondensible organics prior to release to the
atmosphere. The carbon system was charged with 1,500 pounds of
carbon (Remediation Technologies, Inc., 1992). Volatile organic
emissions from the system were monitored in the stack on a
continuous basis .
2.8.2 Pilot Scale Demonstration
Sediments from bins A and B were treated on-site in Buffalo,
New York from October 21 through 31, 1991. Due to freezing
temperatures and heavy snowfall in early November, the thermal
desorption unit and its support equipment were transferred to
RETEC's treatability laboratory in Acton, Massachusetts.
Sediments from bins C and D were treated with the unit set up at
this facility from November 18 through 25, 1991.
Remediation Technologies, Inc. monitored all pertinent process
parameters at routine intervals during the demonstration. This
approach was used to help optimize the removal efficiency of the
thermal desorption demonstration unit as well as to develop data
31
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for the design of full scale equipment. The data collected
included material feed rate, revolutions per minute of the
thermal processor augers, temperature of the heat transfer media
entering and exiting the processor, residence time of the solid
in the processor, temperature of solids entering and exiting the
thermal processor, flow rate of the carrier gas, inlet
temperature of the carrier gas, off-gas temperature, and mass
rates of all process streams. Off-gas concentrations of oxygen
and hydrocarbons were monitored continuously while other data was
recorded at approximately 30 minute intervals during operation of
the unit.
Process temperatures were monitored at 21 locations using
thermocouples. Temperature signals were transmitted to a panel
readout and subsequently recorded on field data sheets
(Remediation Technologies, Inc., 1992). Gas pressures were
monitored in the processing system using magnahelic gauges.
Pressures were monitored within the headspace of the processor
and across the principal components of the off-gas system to
ensure proper operation of the system and to help anticipate
maintenance problems such as poor heat transfer. The flow rate
of inert gas into the processor was monitored by a standard flow
meter while the off-gas flow rate from the thermal system was
monitored in the off-gas stack by measuring the flow with a hot
wire anemometer. The sediment feed rate to the processor was
monitored by recording the volumetric displacement of the feed
system per unit of time in conjunction with associated
measurements of the density of the feed material. The accuracy
of these observations was validated in the field using notations
of the speed and capacities of the processing and cooling augers.
Upon review of the data RETEC determined that there was
significant variability in both the pumping rate and density of
feed material. Therefore, the average material feed rates were
calculated by dividing the total mass of feed material for each
test (weighted in the field) by the duration of time that
material was fed into the processor.
2.8.2.1 Sediment A—
Sediment from bin A was treated in the thermal desorption
unit from October 21 thru October 24, 1991. The material was
processed after mixing with a small amount of Buffalo Harbor
water (2% to 3%) to improve the "pumpability" of the material.
The feed rate and residence time were varied for the feed
material designated Al, A2, and A3. Tables 7A and 7B present
the process data for each treatment run as recorded by RETEC.
Sediment from the three runs, Al, A2, and A3, was treated at feed
rates ranging from 346 to 716 pounds per hour (wet weight) and
residence times ranging from 30 to 90 minutes. The process
temperatures ranged from 933°F to 938°F for the heat transfer
media entering the processor, 902°F to 911°F for the heat
transfer fluid leaving the processor, and 380°F to 535°F for the
treated solids exiting the processor.
32
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TABLE 7A
PROCESS PARAMETER VALUES AS MEASURED BY RETEC, INC.
(English Units)
Run
PARAMETER
Date (1991)
Residence Time (min)
Feed Rate (tbs/hr)
Temperatures (°F)
Heat Transfer Media In
Heat Transfer Media Out
Sediment In
Sediment Out
Inert Off-Gas
Heat Input (BTU/hr)
A1
10/21
90
346
938
911
60
535
917
367,390
A2
10/23
60
502
937
905
60
480
950
435,420
A3
10/24
30
716
933
902
60
380
860
421,820
B1
10/25
45
860
937
908
60
300
230
421,820
B2
10/30
60
644
962
929
60
362
656
449,030
83
10/31
90
334
951
920
60
344
756
421,800
C1
11/18
90
484
921
881
60
392
854
554,280
C2
11/19
60
635
832
804
60
415
974
381,000
C3
11/20
45
862
834
802
60
474
900
435,000
D1
11/21
90
388
888
853
60
367
977
476,250
D2
11/22
60
575
872
843
60
423
965
394,600
D3
11/25
45
724
861
824
60
303
975
503,460
TABLE 7B
PROCESS PARAMETER VALUES AS MEASURED BY RETEC, INC.
(SI Units)
Run
PARAMETER
Date (1991)
Residence Time (min)
Feed Rate (kg/hr)*
Temperatures ("O*
Heat Transfer Media In
Heat Transfer Media Out
Sediment In
Sediment Out
Inert Off-Gas
A1
10/21
90
157
503
488
16
279
492
A2
10/23
60
228
503
485
16
249
510
A3
10/24
30
325
501
483
16
193
460
B1
10/25
45
390
502
487
16
149
110
B2
10/30
60
292
517
498
16
183
347
B3
10/31
90
151
511
493
16
173
402
C1
11/18
90
220
494
472
16
200
457
C2
11/19
60
288
444
429
16
213
523
C3
11/20
45
391
446
428
16
246
482
01
11/21
90
176
476
456
16
186
525
D2
11/22
60
261
467
451
16
217
518
03
11/25
45
328
461
440
16
151
524
* These data are converted from English Units and are rounded to the nearest whole number.
DATA SOURCE: Referenced RETEC, Inc. Report
33
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Some operational problems were encountered during the. processing
of the sediment. Initial feed to the unit was erratic due to
RETEC's unfamiliarity with the peristaltic pump and because the
pump was delivered from the manufacturer with a peristaltic hose
that was not compatible with the sediment material (Remediation
Technologies, Inc., 1992). A consistent flow was established
once the pump hose was changed from a high density polyethylene
to a natural rubber material. In addition, some fouling of the
processor was encountered between the processing of samples A2
and A3. RETEC reported that the fouling was the result of caking
of dried sediments around the processing augers. The processor
was partially disassembled and the caked solids were manually
removed from around the augers.The buildup of dried material was
thought to have been due to the cohesive nature of the fine
grained sediments fed into the processor.
2.8.2.2 Sediment B—
Material from bin B was treated in the thermal desorption
unit from October 25 thru October 31, 1991. The sediment was
processed after mixing with Buffalo Harbor water to achieve a
target moisture content of 45 percent prior to treatment. The
feed rate and residence time were varied for the feed material
designated Bl, B2, and B3. Tables 7A and 7B present the process
data for each treatment run as recorded by RETEC. Sediment from
the three runs, designated Bl, B2, and B3, was treated at feed
rates ranging from 334 to 860 pounds per hour (wet weight) and
process residence times ranging from 45 to 90 minutes. The
process temperatures ranged from 937°F to 962°F for the heat
transfer media entering the processor, 908°F to 929°F for the
heat transfer fluid leaving the processor, and 300°F to 362°F for
treated solids exiting the processor, as measured by RETEC
personnel.
As in the case of the treatment of sediment from bin A, there was
a significant buildup of dried material in the thermal processor.
While treating sediment sample B3 the buildup became so severe
that the processing augers could no longer rotate and a shear pin
on the auger system broke. The thermal system was disassembled,
the caked solids were manually cleaned out, and the shear pin was
replaced.
2.8.2.3 Sediment C—
On November 3 and 4, 1991 a snow storm left approximately 1
foot of snow covering the project area and the air temperature
dropped to between 25 and 30°F. The unprocessed Buffalo River
sediments from bins C and D as well as hydraulic lines on the
thermal desorption unit froze. This made it impossible to
operate the thermal desorption unit or to feed the sediments
through the peristaltic pump into the processor until warmer
temperatures returned. Rather than waiting for warmer
temperatures to return, the Corps of Engineers and Remediation
Technologies, Inc. agreed that the pilot scale demonstration
should be completed at RETEC's indoor treatability facility in
34
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Acton, Massachusetts. During the weeks of November 4 and
November 11, 1991, RETEC personnel demobilized the pilot scale
unit and set the unit up in their Acton facility. They also
transported the untreated sediments from bins C and D from
Buffalo, New York to Acton, Massachusetts.
Sediments from bin C were processed through the thermal
desorption unit on November 18, 19, and 20, 1991. Tap water was
mixed with the sediments to achieve a target moisture content of
approximately 50 percent prior to treatment. The feed rate and
residence time of the sediment in the thermal unit were varied
for the material designated as Cl, C2, and C3. Tables 7A and 7B
present the processed data for each treatment run as recorded by
RETEC. Sediment from the three runs, Cl, C2, and C3, was treated
at feed rates ranging from 484 to 862 pounds per hour (wet
weight) and process residence times ranging from 45 to 90
minutes. The process temperatures ranged from 832°F to 921°F for
the heat transfer media entering the processor, 802°F to 881°F
for the heat transfer fluid leaving the processor and 392°F to
474°F for treated solids exiting the processor.
2.8.2.4 Sediment D—
Sediment from bin D was treated in the thermal unit November
21, 22, and 25, 1991 in Acton, Massachusetts. Tap water was
mixed with the sediments to achieve a moisture content of
approximately 60 percent prior to treatment. The feed rate and
residence time of the sediment in the thermal unit were varied
for the process runs using sediment samples Dl, D2, and D3.
Tables 7A and 7B present the process data for each treatment run
as recorded by RETEC. Sediment from the three runs was treated
at feed rates ranging from 388 to 724 pounds per hour (wet
weight). Process temperatures ranged from 861°F to 888°F for the
heat transfer media entering the unit, 824°F to 853°F for the
heat transfer fluid leaving the processor, and 303°F to 423°F for
the treated solids exiting the processor.
2.9 RESIDUALS MANAGEMENT
Most of the residuals from the pilot scale demonstration
were disposed of by Remediation Technologies, Inc. While
operating in Buffalo, New York, residual solids and liquids from
the bin A and B treated sediments were collected in 55-gallon
drums. Treated solids from the sediment Al run were disposed
within the Corps Confined Disposal Facility. The remaining
treated solids, including the cyclone material, were used in a
solidification/stabilization demonstration. RETEC sealed the
organic condensate in 55-gallon drums and transported it to
Acton, Massachusetts for proper disposal when the thermal unit
was demobilized from Buffalo, New York. The aqueous condensate
was emptied from the 55-gallon drums into the confines of
Confined Disposal Facility Number 4.
35
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All residuals from the treatment of sediments from bins C and D,
as well as the organic condensate from the A and B process runs
performed in Buffalo, were disposed of by RETEC at a licensed
disposal facility in the New England region.
2.10 SOLIDIFICATION OF SOLID RESIDUE
A portion of the residual solids from the treatment process
were solidified/stabilized. The solidification/stabilization
technology immobilizes certain contaminants by binding them into
a concrete-like, leach resistant mass. The formation of the
solidified product is achieved during a hydration reaction in
which free water is bound to the setting agent. The physical and
chemical stability of the resulting product are functions of the
sediment/residual characteristics, type of setting agent, and
additives used. Cement processes reduce the mobility of heavy
metals due to their conversion to insoluble hydroxides or
carbonates because of the elevated pH of cement.
Under the ARCS Program, the Corps of Engineers evaluated
solidification/stabilization at bench-scale for potential
treatment of contaminated sediments from the Buffalo River. The
evaluation was conducted to determine whether physical and
chemical properties of the sediment would be improved. Results
are reported in "An Evaluation of Solidification/Stabilization
Technology for Buffalo River Sediments" (Fleming, Averett,
Chennell, Perry, 1991) and are summarized here. Based on
analyses of the untreated sediment, five metals were selected for
evaluation: chromium, copper, lead, nickel, and zinc.
Initial screening tests for the laboratory were conducted on the
sediment to narrow the range of binder-to-soil ratios to be
prepared in the detailed evaluation. Three binder materials were
evaluated: cement, kiln dust, and lime/fly ash. Based on the
results of the initial screening tests, binder-to-soil ratios
were selected for the detailed evaluation. Specimens were
prepared by mixing sediment and binder materials and molding the
mixture. The specimens were cured for 28 days at 23°C and 98-
percent relative humidity.
Physical tests including unconfined compressive strength (UCS),
freeze/thaw durability, and wet/dry durability were run to
determine if the physical handling properties of the sediment
were improved. Contaminant release tests were conducted to
determine the effectiveness of the binder materials on
immobilization of the contaminants. Based on the results of the
UCS tests, specimens were selected for evaluation of contaminant
release properties. The solidification/stabilization specimens
were subjected to the U.S. Army Engineers Waterways Experiment
Station serial leach test and the toxicity characteristic
36
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leaching procedure (TCLP). The serial leach test results were
compared to the drinking water standards, and the TCLP results
were compared to the regulatory thresholds.
Based on the TCLP results for crushed specimens, the cement and
kiln dust solidification/stabilization processes were effective
in reducing the leachability for lead, nickel, and zinc.
Leachability of copper and chromium was increased by the
processes when compared with untreated sediment for both the TCLP
and the serial leach test. Heavy metal releases from test
specimens may have been increased during the tests by the
destruction of the physical integrity of the specimens. If
physical stabilization of Buffalo River sediment is to be
performed, cement was recommended as the appropriate binder on
the basis of strength, durability, and leachability.
As a result of this investigation it was decided that a Type I
Portland cement would be used for the pilot scale demonstration
and that a binder (cement) to treated solids ratio of from 0.1 to
0.6 would be used. The solidification/stabilization tests were
initiated on October 30 and November 1, 1991. The treated solids
from process runs Bl and B3 were combined and mixed with Type I
Portland cement to achieve a cement to treated solids ratio of
approximately 0.1. A total of 110 pounds of cement were mixed
with 1,000 pounds of treated solids and 380 pounds of water in
two batches in a 9 cubic foot gas powered concrete mixer (Table
8). The resulting mass was placed and vibrated in a 3-foot
diameter sonotube (mold) form for curing. The form was set on
plastic sheeting prior to placement while the top of the sonotube
was covered with plastic sheeting shortly after placement of the
mix.
TABLE 8
SOLIDIFICATION/STABILIZATION MIXES
Nominal Cement Source of Pounds of Material
to Treated Treated Solids Treated Solids Cement Water Total
Solids Ratio (Process Run)
0. 1
0.2
0.4
0.6
Bl, B3
A2
A3
B2
1000
900
950
1036
110
179
376
619
380
355
495
545
1490
1434
1821
2200
37
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The treated solids from process run A2 were mixed with Portland
cement to achieve a cement, to treated solids ratio of
approximately 0.2. A total of 179 pounds of cement were mixed
with 900 pounds of treated solids and 355 pounds of water in two
batches in the concrete mixer. Solids resulting from the
processing of A3 sediment were mixed with cement to achieve a
cement to treated solids ratio of approximately 0.4. Three
hundred seventy six pounds of cement were mixed with 950 pounds
of treated solids and 495 pounds of water in two batches in the
concrete mixer. Residual solids from the processing of B2
sediments were mixed with Portland cement to achieve a cement to
treated solids ratio of approximately 0.6. Six hundred nineteen
pounds of cement were mixed with 1,036 pounds of treated solids
and 545 pounds of water in two batches. In each case the
resulting mass was placed and vibrated in a sonotube form for
curing in a manner similar to that described in the above
paragraph. The plastic sheeting was removed from the top and the
sonotube form was stripped from the four solidified masses 5 to 7
days after mixing operations. The plastic sheeting was then
placed on top of the four masses and later removed after an
additional four weeks of curing in the field.
2.11 EXECUTION AND COSTS
Sediments were dredged from the upper Buffalo River with a
barge mounted crane and transported to CDF No. 4 by Manson
Construction Co. on October 7, 1991. Sediments were screened
through a 0.75 inch wire mesh on October 8 and 9 by RETEC
personnel to remove oversized material. The screened sediments
were then stored in covered 55 gallon drums while RETEC performed
site preparations and mobilized the pilot scale thermal
desorption processor and support eguipment to the site from
October 7 through October 18, 1991. Startup of the desorption
unit occurred on October 21 with sediments being treated on a 5
days per week, one shift per day basis through October 31. In
early November, freezing temperatures and heavy snowfall
necessitated that the treatment unit and its support equipment be
transferred to RETEC's treatability laboratory in Acton,
Massachusetts. The remaining sediments were treated on a one
shift per day, 5 days per week basis with the unit set up at this
facility from November 18 through 25, 1991.
Costs for the entire project were estimated in the work plan to
be $665,500, including the cost of project management,
preparation of a sampling and analysis plan and health and safety
plan, site preparation, sediment excavation and remediation,
project monitoring, including extensive sampling, sample
analysis, and preparation of this report. Actual cost of the
demonstration, shown in Table 9, was approximately $636,000. It
should be noted that laboratory analytical work performed on
samples collected during the demonstration cost more than the
actual remediation of the sediments. This is not uncommon for a
pilot scale demonstration of this nature.
38
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TABLE 9
COST OF THERMAL DESORPTION PILOT SCALE DEMONSTRATION
Activity Cost
Project Management $75,000
Health and Safety Plan 5,000
Sampling and Analysis Plan 15,000
Sediment Excavation (Incl. Misc.
Equip. & Supplies) 15,000
Site Preparation 23,100
Thermal Desorption Demonstration 173,000
Demonstration Monitoring/Sample Collection
(Incl. Stack Gas Monitoring) 65,000
Sample Analysis 225,000
Solidification/Stabilization 5,000
Report Preparation 35,OOP
Total $636,100
2.12 MONITORING
2.12.1 Process Monitoring by Remediation Technologies. Inc.
(RETEC)
Evaluation of this project was conducted by performing
detailed characterization of the contaminated sediment. Sediment
collected from the river was sampled as soon as practical after
placement in the four bins to provide an initial determination of
the organics and heavy metals in the sediment. A second series
of samples was collected following transport and screening to
remove oversized material in order to evaluate losses subsequent
to the sediments being dredged. Material passing the screen was
stored in barrels and became the feed to the thermal processor.
A third set of samples was collected just prior to the material
being fed to the processor. Treated solids discharged from the
processor were sampled for comparison to the feed and
determination of the efficiency of the thermal process in
removing contaminants of concern. Other process residuals were
also characterized to evaluate contaminant losses from the
overall process.
39
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The critical contaminants for the evaluation were PAHs. Other
organic compounds, including PCBs, were also present. Heavy
metals were important contaminants in the sediment, but their
concentrations were not expected to be significantly affected by
the pretreatment and treatment processes. The effectiveness of
the solidification/stabilization process was evaluated on the
basis of changes in leachate quality for the solidified material
compared to the treated solids.
Sediments from the four bins were managed to produce a range of
water contents for the Buffalo River sediment fed to the thermal
processor. One bin of sediments was maintained close to the
water content of the as-dredged sediment and was the first
material fed to the processor. For barrels of sediment from the
three remaining bins, succeedingly increasing amounts of water
were added to the feed. Three operating conditions were run for
each water content, i.e., for each bin of sediment, yielding a
total of 12 runs for the pilot project.
The pilot scale demonstration was conducted by the USEPA's Great
Lakes National Program Office. The U.S. Army Corps of Engineers,
Buffalo District acted as project manager on this demonstration
in support of the USEPA. The District was responsible for
supervision of the project, including coordination with
contractors, and oversight of the field demonstration, including
field sampling. The Corps of Engineers, Waterways Experiment
Station provided technical support to the Buffalo District in
field sampling activities and implementation of the Quality
Assurance Project Plan. Laboratory analytical work was performed
by Battelle Marine Science Laboratory. RETEC was responsible for
collection and recording of all operational data (U.S. Army
Engineer Waterways Experiment Station, 1991).
Remediation Technologies, Inc. monitored all pertinent process
parameters at routine intervals during the demonstration.
Regular monitoring was done to help optimize the removal
efficiency of the thermal desorption demonstration unit and to
develop data for full scale design. The data collected included
feed rate, revolutions per minute of the thermal processor
augers, input and output temperatures of the heat transfer media,
residence time of the solids in the processor, temperature of
solids entering and exiting the thermal processor, carrier gas
flow rate, carrier gas inlet temperature, off-gas temperature,
and mass rates of principal process streams. Off-gas
concentrations of oxygen and hydrocarbons were monitored
continuously, while other data was recorded at approximately 30
minute intervals during operation. A complete presentation of
RETEC's methods and results are given in: "Field Demonstration
of RETEC Thermal Unit for Remediation of Buffalo River Sediments,
Buffalo River Area of Concern," RETEC, Inc., March 1992.
40
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In summary, process temperatures were monitored at 21 locations
using thermocouples. Temperature signals were transmitted to a
panel readout and subsequently recorded on field data sheets
(Remediation Technologies, Inc., 1992). Gas pressures were
measured in the processing system with magnahelic gauges.
Pressures were monitored within the processor headspace and
across the principal components of the off-gas system to ensure
proper operation of the system and to help anticipate maintenance
problems such as poor heat transfer. Inert gas flow rate into
the processor was monitored by standard flow meter while flow
rate in the off-gas stack was measured with a hot wire
anemometer. The sediment feed rate to the processor was
determined by recording the volumetric displacement of the feed
system per unit time and converting to mass flow rate using the
measured density of the feed material. The validity of these
observations was assessed by comparing them against known
capacities of the processing and cooling augers at the associated
operating conditions. Based on these data, RETEC determined that
there was significant variability in both the pumping rate and
density of feed material. Therefore, average material feed rates
were calculated for each run by dividing the total mass of feed
material by the feed duration.
2.12.2 Air Monitoring
2.12.2.1 Air Monitoring by Remediation Technologies, Inc.
(RETEC) —
RETEC, Inc. monitored process exhaust gas for total
hydrocarbon content and for concentration of four specific
volatile hydrocarbons. These measurements were performed as an
instantaneous assessment of process performance, and were used
with moisture data to optimize process efficiency. Total
hydrocarbon concentration was measured using a flame ionization
detector and a propane standard. This result was converted to an
emissions rate using the stack gas flow rate. Overall emissions
ranged from zero to 1178 ppra as propane, with an average of 10
ppm as propane. The average discharge rate was 0.02 pounds per
hour. Average emissions rates represent the total organic
compound emissions for processing Buffalo River sediment under
the operating conditions of the pilot demonstration.
Additionally, specific analyses were performed for benzene,
toluene, ethylbenzene, and xylene (BTEX) using a modified NIOSH
procedure employing activated charcoal tubes. Exhaust
concentrations of benzene averaged 0.61 mg per cubic meter (0.137
grams per hour). Concentrations of ethylbenzene, toluene, and
xylene averaged 0.06, 0.02, and 0.02 mg per cubic meter,
respectively (Table 10). Again, these average rates represent
expected BTEX emissions for thermal desorption of Buffalo River
sediment under conditions of periodic optimization.
Details of RETEC's air sampling procedures and their use in
process optimization are given in "Field Demonstration of RETEC
Thermal Unit for Remediation of Buffalo River Sediments, Buffalo
River Area of Concern," RETEC, Inc., March 1992.
41
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TABLE 10
RESULTS OF VAPOR MONITORING BY RETEC, INC.
I Date: 10/24/91 I Date: 10/30/91 I Date: 10/31/91 I Date: 11/21/9LL Date: 11/22/91 1 Date: 11/25/91
PARAMETERS
Benzene
Ethylbenzene
Toluene
Xylene
Total BTEX
ing/m ff/hr
1.4 0.310
0.04 0.003
NA NA
0.15 0.033
1.6 0.354
mg/m 2/hr
0.57 0.126
NA NA
NA NA
NA NA
NA NA
•s
mg/m ?/hr
0.52 0.115
NA NA
NA NA
NA NA
NA NA
mg/m g/hr
0.44 .098
NA NA
NA NA
NA NA
NA NA
mg/ra ft/hr
0.55 0.122
NA NA
0.13 0.028
NA NA
NA NA
mg/m ?/hr
0.23 0.051
0.09 0.199
NA NA
NA NA
NA NA
NA = Not Analyzed
DATA SOURCE: Referenced RETEC, Inc. Report: Results are for 8 hour time integrated samples averaged over 8 hour gas
flow rate or 8 hour time period as indicated.
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2.12.2.2 Air Monitoring by E-Three, Inc.—
E-Three, Inc. sampled stack emissions for concentration of
total particulates, polychlorinated biphenyls (PCBs), and
polycyclic aromatic hydrocarbons (PAHs). Sampling was performed
in several 2-3 hour increments over a period of 10 days. Data
generated by E-Three, Inc. was not used for on-site process
optimization. Rather, the E-Three data was used to quantify
emissions of semi volatiles and particulates for the process
conditions used by RETEC. Sampling and analytical methods
numbers are presented in Table 11, and a summary of analytical
results is given in Table 12. Results are for time integrated
samples taken over 3 hours and averaged over the number of dry
standard cubic meters (DSCM) of air discharged from the system in
that time. While these emissions are referred to as "air
emissions," the actual composition is not strictly that expected
for air. The processing system is blanketed with nitrogen to
prevent combustion of organic constituents in the sediment, and
the resulting emissions are 7 percent oxygen. Complete test
results are available in "Stack Emission Test Report:
Demonstration Thermal Desorption Project, Buffalo River
Sediments," E-Three, Inc., Buffalo, NY.
2.12.3 Corps of Engineers Monitoring
The Corps of Engineers performed general project oversite
including direction of all contractors involved in field
operations. Additionally, the Corps of Engineers conducted an
intensive sampling and analysis program as described below and as
delineated in the referenced Quality Assurance Project Plan.
Results of this program are summarized in the following text, and
the complete data set for this effort is presented in Appendix B.
Process data was provided by RETEC, Inc., and appears previously
in Table 7A and 7B.
2.12.3.1 Sampling—
The Corps of Engineers sampled solid and liquid streams both
into and out of each process step and submitted these samples to
Battelle Laboratories for analysis. Analytical methods employed
for these analyses are given in Table 13 for sediments and in
Table 14 for water samples (U.S. Army Engineer Waterways
Experiment Station, 1991). The primary intent of this sampling
and analysis program was to determine process stream changes, and
therefore remediation effectiveness, at each stage of the pilot
operation. Other goals for sampling and analysis were to (a)
obtain information for process scaleup, (b) assess reductions in
contaminant concentrations of the sediment during remediation,
and (c) assess effectiveness of cementitious stabilization as a
treatment for process residuals. A process flow diagram
depicting Corps of Engineers sampling points is given in Figure
10.
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TABLE 11
SUMMARY OF AIR SAMPLING AND ANALYTICAL PROCEDURES:
E-THREE/BATTELLE
Parameter
Sampling Method
Analytical Method
Particulates
PCB/PAH
C02, 02, N2
CO
Moisture
Volumetric Flow
Dioxins
EPA Method 5
EPA Method 23
EPA Methods 3 and 3A
EPA Method 10
EPA Method 4
EPA Method 1 & 2
EPA Method 23
Gravimetric
High Resolution GC/MS
Orsat/CEM
GFC-NDIR
High Resolution GC/MS
DATA SOURCE: Referenced E-Three, Inc. Report
TABLE 12A
AIR EMISSIONS OF POLYCHLORINATED BIPHENYLS
IN MICROGRAMS PER DRY STANDARD CUBIC METER
PCB Homolog
Minimum Emissions
ug/DSCM @ 7% 0
Maximum Emissions
ug/DSCM @ 7% 02
Monochlorobiphenyl
Dichlorobiphenyl
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobiphenyl
Octachlorobiphenyl
Nonachlorobiphenyl
Decachlorobiphenyl
<0.33
<0.33
<0.33
<0.66
<0.66
<0.66
<1.67
<3.62
<3.62
<3.62
<5.55
<5.55
<5.55
<9.18
These values are all below detection limits. Detection limits
are varying due to (a) compound - specific nature of detection
limits and (b) solids content of the sample.
TABLE 12B
AIR EMISSIONS OF PARTICULATES IN MICROGRAMS
PER DRY STANDARD CUBIC METER
Minimum Emissions
ug/DSCM @ 7% 02
Maximum Emissions
ug/DSCM @ 7% 0
Particulates
0.0019
0.0027
44
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PAH
TABLE 12C
AIR EMISSIONS OF POLYCYCLIC AROMATIC HYDROCARBONS
IN MICROGRAMS PER DRY STANDARD CUBIC METER
Minimum Emissions Maximum Emissions Average Emissions
ug/DSCM @ 7% 02 ug/DSCM 9 7% 02 ug/DSCM @ 7% 02
Naphtahalene
Acenapthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benz (a) anthracene
Chrysene
Benzo(bjk)f luoranthrene
Benzo(a)pyrene
Indod ,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo(g,h,i)perylene
TOTAL
27.78
0.25
0.78
1.23
8.68
0.84
3.16
1.81
0.36
0.43
0.85
0.21
0.21
0.20
0.23
322.98
3.34
6.61
3.04
129.62
12.89
93.26
34.67
24.30
10.60
19.45
2.42
3.66
0.32
1.45
114.43
1.31
3.13
4.36
42.96
4.61
27.14
13.62
9.05
3.85
6.01
1.12
1.40
1.65
0.80
235.44
TABLE 12D
AIR EMISSIONS OF DIOXINS IN MICROGRAMS
PER DRY STANDARD CUBIC METER
Dioxin
Minimum Emissions
ng/DSCM 9 7% 02
Maximum Emissions
ng/DSCM @ 7% 02
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
0.03480
0.00727
0.00220
0.00304
0.00573
0.00156
0.00122
0.25800
0.26100
0.00347
0.00313
0.00318
0.00373
0.00115
Emissions reported as 2378-TCDD Toxicity Equivalents (i.e., they are
quantitiated based on a 2378-TCDD Standard)
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TABLE 12E
AIR EMISSIONS OF FURANS IN MICROGRAMS
PER DRY STANDARD CUBIC METER
Furan
Minimum Emissions
ng/DSCM @ 7% 02
Maximum Emissions
ng/DSCM @ 7% 02
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HXCDF
123678-HXCDF
234678-HXCDF
123789-HXCDF
1234678-HpCDF
1234789-HpCDF
OCDF
0.0000
0.0000
0.0000
0.0000
0.0003
0.0000
0.0000
0.0000
0.0000
0.0000
0.0013
0.0000
0.3530
0.0838
0.0686
0.0015
0.0217
0.0237
0.0000
0.0000
* Emissions reported as 2378-TCDD Toxicity Equivalents
(EPA 1989)
Zero values in Table 12E were the result of taking total weight
of the compound collected on resin over the 2-3 hour sample
period and dividing by the dry standard cubic meters (DSCM) of
air emitted in that time.
DATA SOURCE: Referenced E-Three, Inc. Report
Processing was done under 12 sets of conditions, each involving 3
to 4 drums of dredged material. Composite samples were taken for
each set of process conditions as follows: For the solid samples
(IS, 2S, 3S, 4S, 7S, 8S on Figure 10), three grab samples were
taken from each of the drums associated with the process
conditions at that point and composited to form one
representative sample. Feed samples were taken from the top,
middle, and bottom of each drum, while samples of treated
sediment and residuals were taken at approximately the beginning,
middle, and end of each run. Each composite was submitted for
analysis of solids, total organic carbon (TOC), mercury,
chromium, lead, oil and grease, PCBs, and 17 individual
polycyclic aromatic hydrocarbons (PAHs). Additionally liquid
samples were taken at the two points where liquid is removed from
the process, namely: a removal point just past the processor
inlet (9L on Figure 10) and a removal point just prior to the
processor outlet (10L on Figure 10). In each case, the removed
liquid was condensed, collected in a receiver, and the receiver
contents for the entire run were well mixed prior to sampling.
Liquid samples were analyzed for the same chemical parameters as
were the solid samples.
Corps of Engineers air sampling was contracted to E-Three, Inc.,
and the resulting analyses were performed by Battelle
Laboratories. No air sampling was performed directly by the
Corps of Engineers.
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TABLE 13
ANALYTICAL PARAMETERS FOR SEDIMENT SAMPLES
Analvsis
PAHs-16 Compounds
bv GC/MS
PCBs
Ctotal Aroclors)
Cr
Cu
Hg
Pb
Total Organic
Carbon
Total Solids
Total Volatile
Solids
_
16 Fractions
Grain Size
Oil and Grease
(Solvent
Extractables)
ARCS
Required
Detection
Limit
ug/g
0.2
0.02
2
2
0.1
2
300
1000
1000
N/A
N/A
Method
NOAA 1985
NOAA 1985
PNL-SP-19B
PNL-SP-19B
MSL-M-11
PNL-SP-19B
EPA 9060
EPA 160.3
EPA 160.4
PSEP 1986
EPA-LLRS-
GROSSE
Battelle
Instrument
Detection
Limit
ug/g
0.02
0.02
1
1
0.02
1
0.10%
noo ug/g)
0.10%
(100 ug/g)
0.10%
dOO ug/g)
1.00%
N/A
Volume
Required
ml
100
100
50
50
50
50
100
50
Container
4 oz
glass
Spex Jar
or
32 oz
plastic
4 oz
plastic
8 oz
plastic
4 oz
glass
References:
NOAA 1985 - NOAA 1985, Nation Oceanic and Atmospheric Administration,
National Status and Trends Program, Standard Analytical Procedures.
. PAHs: GC/MS, using selective Ions mode (S.I.M)
. PCBs: GC/ECD using capillary columns
PNL-SP-19B - Energy Dispersive X-Ray Fluorescence Spectrometry (SOP # from
Battelle Labs)
MSL-M-11 - Cold Vapor Atomic Absorption. (SOP # from Battelle Labs)
EPA 9060, TOC - U.S. Environmental Protection Agency (EPA). 1986. Test
Methods for Evaluating Solid Waste: Physical/Chemical Methods. SW-846.
U.S. Document No. 955-001-00000, USEPA, Washington, D.C.
EPA 160 - U.S. Environmental Protection Agency (EPA). 1983. Methods for
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, March, 1983,
Method 413.2.
PSEP 1986 - Puget Sound Estuary Protocols.
ASTM-D422 - American Society of Testing Materials (ASTM). 1972. Standard
Method for Particle-Size Analysis of Soil D-422. ASTM, Philadelphia,
Pennsylvania.
EPA-LLRS-GROSSE - Procedure supplied by Great Lakes Large Lakes Lab,
"Analysis of Solvent - Extractable Residue from Whole Sediment."
47
-------
TABLE 14
ANALYTICAL PARAMETERS FOR WATER SAMPLES
Analysis
PAHs - 1 6 Compounds
bv GC/MS
PCBs
(total Aroclors)
Cr
Cu
He
Pb
Total Organic
Carbon
|Total Solids
Total Suspended
Solids
pH
Sp. Conductance
Oil & Grease
ARCS
Required
Detection
Limit
ug/g
2
0.01
1
1
0.1
1
1000
1000
1000
Full Range
Full Range
N/A
Method
NOAA 1985
NOAA 1985
PNL-SP-24
PNL-SP-24
MSL-M-24
PNL-SP-24
EPA 415.2
EPA 160.3
EPA 160.1
5520B
Battelle
Instrument
Detection
Limit
ug/1
0.02
0.01
1
1
0.005
1
1000
1000
1000
1.1 me/1
Volume
Required
ml
1000
1000
.
500
.
200
200
200
1000
Container
1000 ml
glass
1000 ml
glass
500 ml
Teflon
60 ml
glass
1000 ml
polv
200 ml
plastic
1000 ml
glass
Additional References:
PNL-SP-24 - Metals and trace elements in water by Inductively Coupled -
Mass Spectrometry (ICP/MS)
MSL-M-27 - Total mercury in water by CVAA
EPA 415.1 - Total Organic Carbon in water.
Method 5520B - "Standard Methods for the Examination of Water and
Wastewater," 18th Edition, AWWA/WPCF.
48
-------
SOLID PHASE SAMPLE —(S)
LIQUID PHASE SAMPLE —(T)
GAS PHASE SAMPLE —(5)
PILOT-SCALE DEMONSTRATION
OF THERMAL DESORPTION
FOR THE TREATMENT OF
BUFFALO RIVER SEDIMENTS
DEMONSTRATION FLOW DIAGRAM
WITH CORPS OF ENGINEERS
SAMPLING POINTS
FIGURE 10
-------
2.12.3.2 Analytical Protocol—
Samples were analyzed using the analytical methods
referenced in Tables 13 and 14. These methods were applied
within the framework of a Quality Assurance Project Plan (QAPP)
prepared by the U.S. Army Corps of Engineers Waterways Experiment
Station. In general, this QAPP provided for replication of 5
percent of all field samples, performance of matrix spikes/matrix
spike duplicates, and processing of all blanks associated with
standard analytical lab practice. Both the analytical
methodology and the quality assurance procedures generally
proceeded per plan as determined by the Waterways Experiment
Station and the Buffalo District Corps of Engineers. Most of the
detection limits for analytes of concern were at or below the
target limits given in Tables 13 and 14. Exceptions were
detection limits for PAHs and PCBs. Detection limits for PAHs
were 0.06 ug/g for sediment (versus the target 0.02 ug/g) and
0.04 ug/1 for water (versus the target 0,02 ug/1). Detection
limits for PCBs met the target values for sediment, but were 0.05
to 0.5 ug/1 for water (versus the target 0.01 ug/1). Detection
limit problems were caused by matrix effects that necessitated
dilution of the samples in question.
Complete results of these analyses and the associated quality
assurance testing are available in "Report of Chemical Analyses:
Volumes 1-3," prepared for the USEPA Great Lakes National Program
Office by Battelle Marine Research Laboratory. Summaries of
these data, and an assessment of process performance based on
these results, appear in subsequent sections of this report.
3.0 RESULTS AND DISCUSSION
3.1 CORPS OF ENGINEERS RESULTS
Reduced analytical data for the Buffalo Thermal Desorption
Pilot Demonstration appear in subsequent sections of this report.
Data is provided separately for each constituent of concern.
Based upon presented results, an assessment is made regarding
process efficiency for removing each chemical contaminant.
3.1.1 Overall Mass Balance
An overall mass balance was performed on solids and liquids
for this process. The intent was to measure the percent of feed
material that could be accounted for after processing (i.e.,
percent closure). Results of this mass balance were reported by
RETEC, and appear in Table 15. Closures of 100 percent ± 15
percent are desirable. For closures in this range, stream
weights can be used with reasonable confidence to track
individual compounds through the system and thus assess treatment
effectiveness.
Based on acceptable closure constraints, all but Run B3 are
suitable runs for determining process performance. Three
additional runs were eliminated from consideration for other
50
-------
TABLE 15
SOLIDS/LIQUIDS MASS BALANCE
Run No.
Al
A2
A3
Bl
B2
a B3
Cl
C2
C3
Dl
D2
D3
Feed
Material fibs)
1896
2010
2150
1355
2175
2180
1640
1905
1940
1515
1150
1630
Treated (b)
Material ribs)
970
1055
1235
845
1850
585
880
955
950
700
480
955
Total
Condensate (Ibs)
765
890
688
620
445
465
840
880
850
950
550
790
Percent
Closure
93
97
89
108
106
48
105
96
93
109
90
107
a. Closure is unacceptable for mass balance calculations
b. This weight includes the weight of the solids which exited the
cyclones.
DATA SOURCE: Referenced RETEC, Inc. Report
reasons. Run Al was considered a startup run, so only a partial
data set was taken. Due to budget constraints, Runs D2 and D3
were archived without performing analytical tests. Thus, all
subsequent data is reported for Runs A2, A3, Bl, B2, Cl, C2, C3,
and Dl.
3.1.2 Solids Content
Total solids data is given in Tables 16A and 16B and
volatile solids data is presented in Table 17. Graphs of these
parameters versus final solids temperatures are given in Figures
11 and 12 (Error bars shown are for the standard error of the
mean). From these data, it is clear that feed material
containing 44-56 percent solids was successfully pumped and dryed
such that final solids content normally exceeded 95 percent.
Maximum sediment temperatures employed to achieve these results
varied from 300°F to 480°F and residence times varied from 30 to
90 minutes.
Because one project goal was to obtain information for design and
operation of a full scale process, it was desired to determine
whether removal efficiencies were a function of any of the
process variables monitored for the study. To assess effects of
process variables, correlation coefficients were determined
relating removal to each measured process parameter. (The
formula used to calculate the correlation coefficient is given in
Appendix A).
51
-------
TABLE 16A
PERCENT TOTAL SOLIDS IN SEDIMENT
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
58.0
63.0
55.4
99.8
95.3
77.1
A3
716
30
380
58.0
60.2
55.0
99.5
97.5
99.6
Bl
860
45
300
55.2
63.2
56.1
98.6
99.1
99.5
B2
644
60
364
55.2
62.0
54.6
99.8
87.1
99.5
Cl
484
90
392
59.8
63.8
52.1
99.8
83.0
98.4
C2
635
60
415
59.8
63.9
50.8
99.9
95.3
N/A
C3
862
45
474
59.8
64.8
48.3
95.2
85.1
99.6
Dl
388
90
367
56.9
58.2
44.6
99.9
94.2
99.7
TABLE 16B
PERCENT TOTAL SOLIDS IN CONDENSATE
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A?
1.1
0.8
A3
1
1
1
I N/A
1
I 0.8
1
Bl
1
1
1
I N/A
1
I 0.8
1
B2
1
1
1
I 0.7
1
| 0.2
1
Cl
0.9
0.2
C2
1
1
1
I 0.5
1
| 0.1
1
C3
1
1
1
I 0.9
1
| 0.1
1
Dl
0.4
0.2
* Process conditions same as for sediment
N/A = Not Analyzed
Highlighted values are average of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
52
-------
TABLE 17
PERCENT VOLATILE SOLIDS IN SEDIMENT
1L
-Cl.
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st cyclone (7s)
Solids from 2nd Cyclone (8s)
346
60
480
6.4
6.0
5.6
3.4
4.7
2.3
716
30
380
6.4
6.0
5.6
4.2
5.4
4.7
860
45
300
6.2
5.4
5.5
3.7
5.1
5.0
644
60
364
6.2
5.4
5.5
4.3
3.8
3.8
484
90
392
5.1
4.9
5.4
4.3
4.9
4.2
635
60
415
5.1
5.3
5.6
3.7
4.9
N/A
862
45
474
5.1
5.5
5.0
4.1
5.2
4.8
388
90
367
5.5
5.4
4.9
3.4
5.1
4.5
% Volatile Solids = (A - Dl x 10Q
WHERE: A = weight of residue after drying at 105"C for 1 hour
D = weight of residue after dried residue has been ignited at 550°C for 1 hour
Highlighted values are the averages of multiple measurements.
calculated using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
N/A = Not Analyzed.
Averages were
53
-------
FIGURE 11
% SOLIDS VERSUS EXIT TEMPERATURE OF SOLIDS
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
100
99.5
to
o
o
»-
*<
99.0
96.5
3J5)
IS)
JO,
(3)
300 350 400 450
EXIT TEMPERATURE OF SOLIDS, °F
500
-------
FIGURE 12
% VOLATILE SOLIDS VERSUS EXIT TEMPERATURE OF SOLIDS
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
5.0
in
o
10
§ 3.0
2.0
(3)
(3)
(3)
(3)
(5)
(5)
(3)
T<3)
300 350 400 450
EXIT TEMPERATURE OF SOLIDS, "F
500
55
-------
A correlation coefficient of ± 1.0 means that process performance
can be perfectly predicted if the value of the process variable
is known. An r value of 0 means that process performance and the
process variable are completely unrelated. (Correlation
coefficients ranging from 0 to +1.0 apply to variables related by
a straight line with a positive slope and correlation
coefficients from 0 to -1.0 apply to variables that are related
by a straight line with a negative slope.) Correlation
coefficient values with an absolute value higher than 0.9 are
usually considered as acceptable for prediction of process
performance. Correlation coefficients relating process
parameters with volatiles removal are given in Table 18.
TABLE 18
CORRELATION COEFFICIENTS FOR VOLATILE SOLIDS REMOVAL
Parameter Correlated with Total
Volatile Solids (TVS) Removal
Correlation Coefficient
Process Temperature
Residence Time
Initial Volatiles Solid Content
0.40
0.40
-0.34
Based on these results, it is clear that some other phenomenon
besides initial liquids content and simple energy input is
dictating extent of drying of sediment and therefore extent of
contaminant removal. It is possible that some threshold energy
input is required before complete removal of these materials is
achieved, and that the threshold was not reached with the
residence times and temperatures employed for this study.
RETEC's thermal desorption process is capable of achieving
maximum sediment temperatures of 700-800°F, at the expense of
throughput rate. Should this process be tried again, it is
suggested that trials at higher temperatures take place.
3.1.3 Metals
An overall material balance was performed on each run for
each metal of concern. A sample calculation is provided for Run
A3, for chromium, as follows:
(a) Adjustment of Measured Stream Weights to a Dry Weight Basis
Mass of Input:
(2150 Ibs) x (0.550 Ibs drv solids) x (0.454 kg) = 537 kg dry solids
Ib Ib
Mass of Output/Solid Stream (Average percent solids in treated solids
plus residue from cyclones):
(1235 Ibs) x (0.995 Ibs drv solids) x (0.454 kg) = 557 kg dry solids
Ibs Ib
56
-------
Mass of Solid Output in Liquid Stream:
(688 Ibs liquid) x (0.008 Ib solids) x (0.454 kg) = 2.5 kg dry solids
Ib liquid Ib
(b) Material Balance on Chromium for Run A3
Input:
(537,000 g solids) x (68 x 10"fe a Cr) = 36.5 g Cr
g solids
Since it is not known what percent of total solids came from the
cyclones (they were combined and then analyzed), the following is
assumed for these calculations:
cyclone 1: 4%
cyclone 2: negligible
Overall concentration of processed solids is therefore:
0.96(61) + 0.04(148) = 65 ug/g
Where 61 ug/g and 148 ug/g are analytical values
Cr in Treated Solids:
(557,000 g) x (65xlO~6 a Cr) = 36.2 g
g
Cr in Condensate Solids:
(2,500 g) f!48xlO"6 a Cr) = 0.37 g (negligible)
g
Cr in Condensate:
(688 Ibs) x (0.454 ka) = 312 kg
Ib
(312 kg) x (1L) x (14.200 x 10"6 cr Cr) =4.4 grams
kg L
Percent Removed from Sediment:
(36.5 g - 36.2 q) x 100 = 0.8% removal
36.5 g
Analytical results for metals are summarized in Tables 19A and
19B thru 22A and 22B. From these results, it is clear that
removal levels are somewhat metal specific. Copper, lead, and
chromium are discussed together because they behave similarly
under conditions employed for this study. Mercury is discussed
separately because its behavior is distinctly different from the
other metals.
Copper. Lead, and Chromium
For copper, lead, and chromium, residue concentrations in
ug/g did not change appreciably from those in the feed although
57
-------
TABLE 19A
LEAD IN SEDIMENT
(ug/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
72.2
52.4
53.7
52.1
58.9
48.8
A3
716
30
380
72.2
52.4
52.4
52.7
56.7
48.0
Bl
860
45
300
49.3
58.2
64.3
65.7
65.1
58.4
B2
644
60
364
49.3
58.2
61.7
67.0
67.0
64.5
Cl
484
90
392
88.8
62.3
68.4
70.6
83.8
59.7
C2
635
60
415
88.8
62.3
71.9
67.2
70.7
N/A
C3
862
45
474
88.8
62.3
56.3
58.3
70.4
61.7
Dl
388
90
367
49.7
62.3
73.5
64.7
63.6
71.8
TABLE 19B
LEAD IN CONDENSATE
(Filtered)
(ug/L)
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A2
1 1
1 1
1 1
| N/A |
1 1
1 2.97|
1 1
A3
1
1
1
N/A |
1
1.19 |
1
Bl
1
1
1
N/A |
1
3.56 |
1
B2
1
1
1
N/A |
I
2.37 |
1
Cl
1
1
1
N/A |
1
1.78 |
1
C2
N/A
14.0
C3
N/A
17.8
Dl
N/A
8.90
N/A Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
58
-------
TABLE 20A
CHROMIUM IN SEDIMENT
(ug/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
73
60
47
70
137
84
A3
716
30
380
73
60
68
61
148
88
Bl
860
45
300
63
51
47
56
129
121
B2
644
60
364
63
51
58
44
106
77
Cl
484
90
392
80
71
73
67
136
129
C2
635
60
415
80
71
59
58
129
N/A
C3
862
45
474
80
71
69
62
140
140
Dl
•388
90
367
74
60
55
62
112
118
TABLE 20B
CHROMIUM IN CONDENSATE
(Filtered)
(ug/L)
Run
Number A2 A3 Bl
1
SAMPLE POINTS * |
After 1st
After 2nd
1
1 1
1 1
1 1
Condenser (9L) | N/A | N/A | N/A
1
Condenser (10L) 4
1 1
2 2.9 | 2.52
1
B2
1
1
1
I N/A
1
I 1.76
1
Cl
1
1
1
I N/A
1
| 2.78
1
C2
1
1
1
| N/A
1
I 1.80
1
C3
N/A
1.01
Dl
1
1
1
I N/A
1
I 1.64
1
N/A Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
59
-------
TABLE 21A
COPPER IN SEDIMENT
(ug/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
46.2
45.8
41.1
38.2
51.3
42.3
A3
716
30
380
46.2
45.8
40.6
41.3
47.1
43.1
Bl
860
45
300
41.0
43.0
37.6
45.7
48.2
46.2
B2
644
60
364
41.0
43.0
43.0
45.6
46.8
47.1
Cl
484
90
392
56.8
47.8
45.3
58.0
54.8
62.1
C2
635
60
415
56.8
47.8
48.2
48.8
56.1
N/A
C3
862
45
474
56.8
47.8
47.2
45.4
62.4
52.5
Dl
388
90
367
37.7
45.0
44.8
47.6
51.3
53.7
TABLE 21B
COPPER IN CONDENSATE
(Filtered)
(ug/L)
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A2
N/A
830
A3
1
1
1
I N/A
1
| 410
1
Bl
1 1
1 1
1 1
I N/A |
1 1
1 340 |
1 1
B2
1
1
1
N/A |
1
450 |
1
Cl
1
1
1
N/A |
1
720 |
1
C2
N/A
120
C3
1
1
1
N/A |
1
70 |
1
Dl
N/A
755
N/A Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
60
-------
TABLE 22A
MERCURY IN SEDIMENT
.(ug/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
0.18
0.19
0.17
0.00
0.15
0.02
A3
716
30
380
0.18
0.19
0.18
0.05
0.12
0.04
Bl
860
45
300
0.17
0.21
0.20
0.11
0.13
0.12
B2
644
60
364
0.17
0.21
0.20
0.00
0.10
0.02
Cl
484
90
392
0.34
0.20
0.20
0.07
0.32
0.30
C2
635
60
415
0.34
0.20
0.21
0.05
0.22
N/A
C3
862
45
474
0.34
0.20
0.18
0.15
0.49
0.06
Dl
388
90
367
0.11
0.21
0.19
0.01
0.21
0.03
TABLE 22B
MERCURY IN CONDENSATE
(Filtered)
(ug/L)
Run Number
_A2_
_A3_
Bl
_B2_
_C_2_
I I I I I I I I
SAMPLE POINTS * I I I I I I I I
I I I I I I I I
After 1st Condenser (9L) |(44.07)| 3.26 | N/A | 5.28 | 9.30 | 2.16 | 0.01 | 3.20
I I I I I I I I
After 2nd Condenser (10L) | 2.50 | 4.00 | 0.95 | 1.44 | 1.34 | 3.66 | 1.81 | 3.37
I I I I I I I I
N/A Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
61
-------
concentrations of lead and chromium decrease significantly from dredging
to screening. Although not determined experimentally, it is postulated
that some of the metals precipitated and adhered to the side-walls of
the storage drum. During treatment, all three metals tend to remain
with the treated residue, and are thus found either in the bulk of the
treated residue or in the treated solids captured by the cyclones. For
copper and lead, concentration of the cyclone solids is approximately
the same as concentration of the bulk residue. For chromium, the
concentration is greater in the cyclone solids than in the bulk residue,
suggesting that chromium tends to associate with the finer particulates.
Concentrations of Cu, Pb, and Cr in condensate are negligible. In
summary, copper, chromium and lead tend to remain with the solids and
are potential candidates for stabilization.
One of the goals for this study was to assess contaminant losses during
processing. For this reason, a mass balance was performed on each metal
for each process step to determine fate of the metals that were removed
by processing. That is, if the constituent was desorbed from the
residue, where did it go and how must it be captured to prevent further
environmental contamination? A sample mass balance calculation is given
in Appendix A. Table 23 summarizes the mass balance results for Cu, Pb,
Cr, and Eg.
From these results it is clear that the majority of these metals remain
with the residue. As can be seen from these results, mass balance
closures are variable. Sometimes all material is not accounted for,
while at other times the output of key constituents of concern appears
to exceed the input. There are several reasons why this is true.
(1) Most constituents of concern for this project were
present in extremely small quantities. For example,
the total quantity of chromium being tracked through
the process for an entire run was in the range of 50
grams. For such small contaminant quantities, the sum
of the extremely small errors inherent in the
analytical procedures comprises a significant
percentage of the total amount present.
(2) Individual weights of the solid streams were not
taken, rather all solids were combined and a single
weight was obtained. Since compositions of these
individual streams were not the same, the act of
combining these streams resulted in an approximate
rather than an exact material balance.
(3) Air emissions analysis did not include analysis
for metals, thus metal losses into the atmosphere or
within the carbon adsorber were not quantified.
Indeed, the carbon adsorber is a sink that was not
accounted for in the sampling and analysis program.
-------
TABLE 23A
SUMMARY OF CALCULATIONS
CHROMIUM
< GRAMS OUT >
PERCENT
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
No
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
No
GRAMS IN
23.7
36.5
16.2
31.3
28.3
25.9
29.3
16.9
significant
GRAMS IN
20.7
21.8
13.0
23.1
17.5
21.1
20.0
13.8
significant
RESIDUE CONDENSATE
34.8 5.2
36.2 4.4
22.3 0.5
39.4 0.0
27.9 0.3
26.4 0.2
26.7 0.4
20.3 0.3
AVG
change
TABLE 23B
SUMMARY OF CALCULATIONS
COPPER
< GRAMS OUT >
RESIDUE CONDENSATE
18.4 10.3
23. O 2.2
17.3 0.2
38.5 0.0
23.0 1.4
21.2 0.9
18.9 0.8
15.2 0.3
AVG
change
REMOVED
0
0.8
0
0
1.4
0
8.8
0
1.4
PERCENT
REMOVED
11.1
0
0
0
0
0
5.5
0
2.0
63
-------
TABLE 23C
SUMMARY OF CALCULATIONS
LEAD
< GRAMS OUT >
PERCENT REMOVED
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
No
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
GRAMS IN
27.1
28.1
22.2
33.3
26.5
31.6
23.9
22.6
sicrnif leant
GRAMS IN
.086
.094
.070
.107
.078
.094
.074
.057
RESIDUE CONDENSATE
25.0 5.1
29.5 2.2
24.7 0.0
56.1 0.0
28.3 0.3
29.1 0.1
24.2 0.1
20.5 0.2
chancre
TABLE 2 3D
SUMMARY OF CALCULATIONS
MERCURY
< GRAMS OUT >
RESIDUE CONDENSATE
.005 0.03
.028 0
.042 0
0 0
.030 0
.010 0
.067 0
.007 0
FROM SEDIMENT
7.7
0
0
0
0
7.9
0
9.3
AVG 3 . 1
PERCENT REMOVED
FROM SEDIMENT
94.1
70.2
40.0
100
61.5
89.4
9.5
87.7
AVG
69.2
64
-------
(4) The process equipment used for this demonstration
was, of necessity, portable equipment that is often
transported, disassembled, and reassembled. For this
reason, areas near seals were not as air-tight as they
tend to be when assembly and disassembly are
infrequent. Some fine particulate losses were observed
at the seal where the conveyor dome bolts to the
conveyor body. Since the constituents of concern
tended to be either volatile or associated with fine
particulates, these small losses could affect the
material balance. It must be emphasized that losses of
this nature did not result in measurable discharges of
pollutants to the environment. The contaminant input
to the process equipment was so small that is was
barely measurable, thus losses that affected material
balance closures were trace amounts indeed.
For future work, it is recommended that air emissions losses for
metals be performed and that process streams are weighed separately
before they are combined for disposal. This should help improve mass
balance closure somewhat and should permit calculation of air
emissions. As for the other sources of error, problem (4) will be
greatly minimized for full scale, permanently installed equipment.
The impact of problem (1) can be minimized for highly contaminated
sediments, but cannot be corrected by process methodology.
Mercury
Following processing, the bulk of the treated residue was free of
mercury as were the solids from the second cyclone and the condensate.
Mercury content of solids from the first cyclone was approximately the
same as the untreated solids. Based on mass balances, however, an
average of 79 percent of the mercury in the feed was unaccounted for
after processing. Reasons why the fate of mercury is largely unknown
are the same as reasons why closure was not obtained for chromium,
copper, and lead. As for these other metals, closure can be somewhat
improved by weighing each process stream and by quantifying air
emissions. Air emissions monitoring will be even more important for
mercury, however, because it is a liquid at room temperature and has a
relatively high vapor pressure. Again, equipment leaks and errors due
to low initial concentrations are inherent in the process and cannot
be eliminated in a pilot study of this nature.
3.1.4 Polycyclic Aromatic Hydrocarbons (PAHs)—
Concentrations of 17 individual PAHs were measured both before
and after processing, and an attempt was made to assess both removal
efficiency and ultimate fate of the removed materials. (Although not
confirmed experimentally, it is likely that PAH concentrations
increased between dredging and screening due to concentration effects
of liquid evaporation.) Where a concentration was reported as "less
than detection limit," the detection limit itself was the
concentration used in the summation. This approach was used to assure
that sediment disposal questions addressed for process scaleup would
provide maximum environmental protection. To facilitate this
analysis, individual PAH results were summed in two groups.
65
-------
Low molecular weight PAHs, i.e., those
containing < 3 aromatic rings (naphthalene,
acenaphthylene, acenaphthene, fluorene, phenanthrene,
anthracene).
High molecular weight PAHs, i.e., those
containing > 3 aromatic rings (fluoranthene, pyrene,
benzo(a)anthracene, chrysene, benzo(b)fluoranthene,
benzo(k)fluoranthrene, benzo(a)pyrene,
indeno(1,2,3-cd)-pyrene, dibenzo(a,h)-anthracene, and
benzo(g,h,i)-perylene) .
Individual compounds were grouped this way primarily because many PAHs
with > 3 aromatic rings are either known or suspected carcinogens,
thus their fate and removal efficiencies are of particular interest.
PAH removal efficiencies are discussed by group, as follows:
Low Molecular Weight PAHs (LMW PAHs)
Results of low molecular weight PAH removal are given in Tables
24A and 24B. A graph of LMW PAH concentration versus final solids
temperature is given in Figure 13 (Error bars shown are for standard
error of the mean). From these data it is determined that a range of
45 to 90 percent of the PAHs with < 3 aromatic rings were removed from
the feed material as a result of thermal desorption. Correlation of
removal with process temperatures was not significant, as the
correlation coefficient relating the two variables was 0.00. It is
not known whether a larger energy input would remove the remaining LMW
PAHs from the sediment. Future work involving low temperature thermal
desorption should include some higher temperatures in order to assess
the effect of this process parameter.
As for fate of the removed PAHs, concentration of LMW PAHs in the
solids captured by the cyclones is approximately that found in
the unprocessed feed. Negligible amounts of LMW PAHs are found
in the condensate (average = 0.14 ug/g) and in the air emissions
(range is 41.1-213.6 ug/DSCM). Net result is that approximately
74 percent of the PAHs originally present in the feed are not
accounted for by mass balance (Table 26A). Closure was not
obtained for LMW PAHs. The first three reasons for low percent
closure given in section 3.1.3 apply here as well. Additionally,
it is speculated that much of the unaccounted-for PAHs sorbed to
the carbon. The LMW PAH compounds have an activated carbon:
water partition coefficient (Pac) of 10E4.7 to 10E6.8
(Verscheuren, 1983). This range of Pac values suggests a strong
tendency for carbon to adsorb airborne PAHs from the exhaust air.
For any future work of this nature, it would be well to attempt
identifying and quantifying the chemicals adsorbed by the carbon
system. Desorption of these materials and their subsequent
quantification may be impractical, but if investigation of the
problem results in disclosure of a practical methodology, the
resulting data will be valuable.
66
-------
TABLE 24A
LOW MOLECULAR WEIGHT (<. 3 RING)
PAHs IN SEDIMENT
(ng/g Dry Weight)
Run Nvrober
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
791
1538
1124
122
1947
1105
A3
716
30
380
791
990
1177
210
838
327
Bl
860
45
300
926
950
842
349
1417
1430
B2
644
60
364
926
1170
1367
107
1625
613
Cl
484
90
392
1390
1577
1428
211
N/A
1663
C2
635
60
415
1390
1221
1164
260
822
N/A
C3
862
45
474
1390
1221
1039
425
4493
369
Dl
388
90
367
937
9994
2018
102
2689
576
TABLE 24B
LOW MOLECULAR WEIGHT U 3RINGS)
PAHs IN CONDENSATE
(ug/L)
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A2
215
230
A3
361
147
Bl
N/A
209
B2
20
68
Cl
149
N/A
C2
205
55
C3
45
159
Dl
65
35
* Process conditions same as for sediment
N/A Not Analyzed
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
67
-------
FIGURE 13
CONCENTRATION OF LOW MOLECULAR WEIGHT PAH* IN SEDIMENT
VERSUS EXIT TEMPERATURE OF SOLIDS
.8
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
500
400
o
300
o>
o>
200
z
UJ
o
100
(3)
(5)
(A)
•I
(3)
(6)
1,3,
(3)
300 350 400 450
EXIT TEMPERATURE OF SOLIDS. °F
500
68
-------
High Molecular Weight PAHs (HMW PAHs)
High molecular weight PAH removal results are given in
Tables 25A and 25B. A graph of HMW PAH concentration versus
final solids temperature is given in Figure 14 (Error bars shown
are for standard error of the mean). Based on these results, it
is concluded that 72 percent of all PAHs with carcinogenic
potential have been removed by this process (Table 26B). As with
other contaminants of concern, HMW PAH removal does not correlate
well with maximum sediment temperature. The correlation
coefficient relating these variables was 0.00. As was stated for
LMW PAH removal, effect of higher temperature on removal should
be assessed for future work.
As for the fate of removed HMW PAHs, concentration of these
materials in the first cyclone is approximately that found in the
unprocessed feed. Concentration of HMW PAHs in the second
cyclone is between that in the unprocessed feed and that in the
bulk of the treated residue. Negligible amounts of HMW PAHs are
found in the condensate (average = 0.15 ug/g) and in the air
emissions (range is 8.9E-07 to 2.3E-05 ug/DSCM). Net result is
that 71.6 percent of the HMW PAHs in the feed are unaccounted-for
by the overall mass balance (Table 25B). The same reasons for
low percent closure that applied to LMW PAHs apply here, except
that tendency to sorb to carbon is stronger for the HMW PAHs (Pac
for HMW PAHs is 10E6.5 to 10E7.0).
Total PAHs
Total PAH removal results are given in Tables 27A and 27B.
Based on these results, from 43-94 percent of the total PAH
contaminants were removed by the thermal desorption process.
Fate of these materials has been discussed previously under
sections pertaining to Low Molecular Weight PAHs and High
Molecular Weight PAHs and is not repeated here. Tables showing
removals of specific PAHs are given in Appendix A.
3.1.5 Solvent Extractables (SE)
Results of solvent extractables removal, as measured by
standard oil and grease analysis, are presented in Tables 28A and
28B. A graph of solvent extractable concentration versus solids
temperature is given in Figure 15. Error bars shown are for
standard error of the mean. From these data it is determined
that 17-86 percent of the oil and grease was removed from the
residue, with an average removal of 68 percent. SE removal did
not correlate well with maximum sediment temperature, as the
correlation coefficient relating temperature and removal was
-0.45. It is not known whether use of higher temperatures could
improve removal. While low correlation of removal with
temperature was true for temperatures < 480°F, it may be true
that some specific additional energy input is required before
removal of SE can occur.
-------
TABLE 25A
HIGH MOLECULAR WEIGHT (>3 RINGS)
PAHs IN SEDIMENT
(ng/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
5424
7860
6990
119
4354
1588
A3
716
30
380
5424
6325
5529
1425
8811
3938
Bl
860
45
300
6604
5787
5621
1664
11,679
2300
B2
644
60
364
6604
7187
6502
61
7610
4349
Cl
484
90
392
7652
7519
7198
1608
N/A
6943
C2
635
60
415
7652
6600
5985
1865
8019
N/A
C3
862
45
474
7652
6804
5952
3549
21,178
3043
Dl
388
90
367
6479
41,871
9535
450
25,499
6744
TABLE 25B
HIGH MOLECULAR WEIGHT (>3 RINGS)
PAHs IN CONDENSATE
(ug/L)
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A2
1
1
1
I 156
1
I 268
1
A3
235
190
Bl
1
1
1
N/A |
1
245 |
1
B2
7
59
Cl
1
1
1
129 |
1
N/A |
1
C2
218
75
C3
82
220
Dl
1
1
1
1 HI
1
1 42
1
N/A Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
70
-------
TABLE 26A
SUMMARY OF CALCULATIONS
LOW MOLECULAR WEIGHT PAHs
< MILLIGRAMS OUT >
PERCENT
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
MGMS IN
568
632
290
737
554
511
442
620
RESIDUE
93
82
145
141
107
122
242
65.1
CONDENSATE
0.08
0.11
0.06
0.00
0.06
0.08
0.02
0.02
AVG
REMOVED
83.7
87.1
50.0
80.9
80.6
76.1
45.3
89.5
74.2
TABLE 26B
SUMMARY OF CALCULATIONS
HIGH MOLECULAR WEIGHT PAHs
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
MGMS IN
3530
2969
1939
3504
2793
2627
2487
2927
MILLIGRAMS OUT >
RESIDUE CONDENSATE
138
958
782
305
725
914
1436
734
0.06
0.07
0.07
0.00
0.05
0.09
0.03
0.03
AVG
PERCENT
REMOVED
96.1
67.7
59.7
91.3
74 . 1
65.2
42.2
74.9
71.4
71
-------
FIGURE 14
CONCENTRATION OF HIGH MOLECULAR WEIGHT PAHS IN SEDIMENT
VERSUS EXIT TEMPERATURE OF SOLIDS
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
2500
2000
x
o
Ld
3C
g 1500
cn
c
z
g 1000
<
o:
LJ
o
§ 500
o
(5)
(3
(3)
(5)
(3)
J(6)
I
(3)
300 350 400 450
EXIT TEMPERATURE OF SOLIDS, °F
500
72
-------
TABLE 27A
TOTAL PAHs IN SEDIMENT
(ng/g dry weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc . (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
6215
9398
8114
241
6301
2693
A3
716
30
380
6215
7315
6706
1635
9649
4265
Bl
860
45
300
7530
6737
6463
2013
13096
3730
B2
644
60
364
7530
8357
7869
168
9235
4962
Cl
484
90
392
9042
9096
8626
1819
N/A
8606
C2
635
60
415
9042
7821
7149
2125
8841
N/A
C3
862
45
474
9042
8025
6991
3974
25671
3412
Dl
388
90
367
7416
51865
11553
552
5238
7320
TABLE 27B
TOTAL PAHs IN CONDENSATE
(ug/L)
Run Number
A2
A3
Bl
B2
_CL
_C2_
_C3_
Dl
I I I I
SAMPLE POINTS * I I I I
I I I I
Liq. from 1st Condenser (9L) | 371 | 596 | N/A | 20
I I I I
Liq. from 2nd Condenser (10L)| 498 | 337 | 454 | 127
I I I I
I I I
I I I
I I I
278 | 423 | 127 | 176
I I I
N/A | 130 | 379 | 77
N/A - Not Analyzed
* Process conditions same as for sediment
Highlighted values are averages of multiple (3-5) measurements.
DATA SOURCE: Referenced Battelle Report
73
-------
TABLE 28A
SOLVENT EXTRACTABLES IN SEDIMENT
(ug/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
1415
1820
2282
234
2391
696
A3
716
30
380
1415
1766
2250
550
2443
1901
Bl
860
45
300
1619
2006
2056
474
3770
1899
B2
644
60
364
1619
2082
1754
220
1231
449
Cl
484
90
392
2261
3995
2109
562
N/A
2539
C2
635
60
415
2261
1761
2011
510
2416
N/A
C3
862
45
474
2261
2399
4254
3618
4389
646
Dl
388
90
367
1707
2416
2391
646
5368
965
TABLE 28B
SOLVENT EXTRACTABLES IN CONDENSATE
(mg/L)
Run Number
.A2.
.A3.
_B2_
_CJ_
C3 Dl
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
I I I I I
I I I I I
I I I I I
| 284 | 112 | N/A | 62 | 90
I I I I I
| 110 | 214 | 29 | 70 | N/A
I I I I _ I
82
30
113 | 57
I
16 | 71
I
* Process conditions same as for sediment
N/A - Not Analyzed
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
74
-------
FIGURE 15
CONCENTRATION OF SOLVENT EXTRACTABLES IN SEDIMENT
VERSUS EXIT TEMPERATURE OF SOLIDS
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
3000
2500
x
o
UJ
cc
o
0>
X
2000
z 1500
O
tr
i—
5 1000
o
z
o
o
500
(5)
(5
(3)
(3)
(3)
300 350 400 450
EXIT TEMPERATURE OF SOLIDS. °F
500
-------
As for the fate of oil and grease, it tends to be concentrated in the
fines captured by the first cyclone. Still, 68 percent of the removed
oil and grease is unaccounted for (Table 29). It is known that
negligible amounts appear in the condensate and in the fines from the
second cyclone, however, amounts sorbed on carbon and amounts in air
emissions were not quantified.
Because solvent extractables analysis is a cheap, relative easy
measurement, the possibility of using solvent extractables removal as a
surrogate parameter to predict removal of polycyclic aromatic
hydrocarbons was considered. If correlation between SE removal and PAH
removal were high, a single measurement could replace 16 individual
measurements for estimating PAH removal. Using the calculation protocol
in 6.2.2.2, the correlation coefficient relating SE removal and total
PAH removal was 0.77. This value suggests that use of SE removal as a
surrogate parameter for PAH removal may be possible. Since 80 percent
of solvent extractables are unaccounted for in the material balance,
however, this concept requires further investigation.
3.1.6 Total Organic Carbon (TOC)
Total organic carbon is a surrogate parameter that includes all
organic carbon oxidizable by persulfate in the presence of UV light.
The oxidized carbon is thus quantified by measuring the evolved carbon
dioxide. Given this definition, it is clear that the total organic
carbon (TOC) measured in the sample represents the carbon from: SE,
PAHs, PCBs, pesticides, other (unidentified) semivolatiles, and
volatiles (in untreated material). In addition, some portion of the
naturally occurring humic and fulvic acids will oxidize during the time
of the analytical test run, and this portion of the organic acids will
contribute to total measured carbon. (While humic and fulvic acids are
theoretically all oxidizable, the typical Dohrmann instrument will "time
out" before the oxidation is complete). Effect of thermal desorption on
TOC is given in Tables 30A and 3OB. A graph of TOC concentration versus
final solids temperature is given in Figure 16. (Error bars shown are
for standard error of the mean.)
Removals of TOC ranged from 5 percent to 35 percent, indicating that
most of the compounds contributing to TOC (Table 31) were not removed at
the process temperatures employed. TOC was examined as a potentially
predictive surrogate parameter for several classes of organic compounds.
A reasonably large correlation coefficient relates removal of HMW PAHs
and TOC removal, as evidenced by the following correlation coefficients
(r). Caution must be exercised in using TOC removal to predict HMW PAH
removal, however, because 85 percent of the PAHs were removed with only
25 percent of the TOC.
76
-------
TABLE 29
SUMMARY OF CALCULATIONS
SOLVENT EXTRACTABLES
< GRAMS OUT >
PERCENT
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
GRAMS IN
1152
1208
1184
1137
818
883
1808
734
RESIDUE
163
349
229
218
224
254
1500
253
CONDENSATE
113
NO DATA
8
12.5
0
0
0
0
AVG
REMOVED
85.9
71.2
80.7
80.8
72.6
71.2
17.1
65.5
68.1
77
-------
TABLE 30A
TOTAL ORGANIC CARBON IN SEDIMENT
(mg/g Dry Weight)
Run Number
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
A2
346
60
480
18.6
18.4
18.6
12.1
14.8
10.4
A3
716
30
380
18.6
19.0
19.0
14.7
17.2
14.7
Bl
860
45
300
18.4
18.2
18.9
14.2
17.1
16.9
B2
644
60
364
18.4
18.7
19.1
10.3
15.9
15.3
Cl
484
90
392
17.7
18.0
18.3
15.2
20.6
14.6
C2
635
60
415
17.7
17.7
18.0
15.4
16.6
N/A
C3
862
45
474
17.7
18.4
17.5
16.6
20.5
15.9
Dl
388
90
367
17.6
18.2
18.5
13.2
18.4
15.3
TABLE 3OB
TOTAL ORGANIC CARBON IN CONDENSATE
(mg/g liquid)
Run Number
SAMPLE POINTS *
After 1st Condenser (9L)
After 2nd Condenser (10L)
A2 A3
1 1 1
1 1 1
1 1 1
1 1.58| 1.58 |
1 1 1
I .85| .51 |
1 ! 1
Bl B2
.85
.53
1
1
1
.90 |
1
-75 |
1
Cl
1
1
1
.83 |
1
.28 |
1
C2
.72
.25
C3
1
1
1
1 -43
1
1 -17
1
Dl
.70
.37
* Process conditions same as for sediment
N/A Not Analyzed
Highlighted values are averages of multiple measurements.
using 3-5 individual measurements.
DATA SOURCE: Referenced Battelle Report
Averages were calculated
78
-------
FIGURE 16
TOC (mg/g SOLIDS) VERSUS EXIT TEMPERATURE OF SOLIDS
(NUMBERS IN PARENTHESES ARE NUMBERS OF DATA POINTS
FROM WHICH THE STANDARD ERRORS WERE CALCULATED)
zuuu
i- 1500
X
o
UJ
>_
cr
Q
en 100°
X
g1
z
o
o
i- 500
' T-3> -ll'"1'3'
I.B,
1,3,
1-5,
300 3.50 400 450
EXIT TEMPERATURE OF SOLIDS, °F
500
79
-------
TABLE 31
SUMMARY OF CALCULATIONS
TOC
< LBS OUT >
PERCENT
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
LBS
18.
23.
18.
19.
18.
18.
17.
18.
IN
7
3
9
1
3
0
5
5
RESIDUE
12
12
14
10
15
15
16
13
.1
.5
.2
.2
.2
.4
.6
.2
CONDENSATE REMOVED
1
0
NO
0
0
0
0
0
.4
.4
DATA
.3
.5
.4
.3
.5
AVG
35.3
33.5
24.9
46.6
16.9
14.4
5.1
28.7
25.7
Organic Material r
LMW PAHS 0.58
HMW PAHs 0.81
Total PAHS 0.77
Solvent Extractables 0.71
Fate of TOC is not discussed here, as the "fate" of a surrogate
parameter is not a meaningful concept. What should be emphasized
is that it was possible to account for an average of 77 percent
of the initial TOC and that most of it remained with the
sediment.
3.1.7 Polychlorinated Biphenyls (PCB)
Analyses were performed before and after processing for four
commercial mixtures of PCB (Aroclors): 1242, 1248, 1254, 1260.
These are the Aroclors that could be present in the Buffalo River
based on site history, thus a total of the individual
concentrations of these Aroclors is considered to be total PCB.
Total PCB data are presented in Tables 32A and 32B. Data in
Tables 32A and 32B are limited primarily to information
associated with performance of the thermal processor itself; data
associated with more remote parts of the process were not
analyzed (N/A) due to cost constraints.
Percent PCB removals were calculated using data in Table 32, and
these results are presented in Table 33. Removals ranged from 0
to 100 percent. No correlation was observed between maximum
sediment temperature and PCB removal (r = -0.05).
80
-------
TABLE 32A
TOTAL PCB IN SEDIMENT
(ng/g dry weight)
Run Number A2 A3 Bl B2 Cl C2 C3 Dl
PROCESS CONDITIONS
Feed Rate Ibs/hr
Residence Time min.
Max. Sediment Temp. °F
SAMPLE POINTS
After Dredging (Is)
After Screening (2s)
Before Thermal Proc. (3s)
After Thermal Proc. (4s)
Solids from 1st Cyclone (7s)
Solids from 2nd Cyclone (8s)
346
60
480
N/A
N/A
ND
ND
ND
ND
716
30
380
N/A
N/A
ND
ND
402
67
860
45
300
N/A
ND
184
94
589
156
644
60
364
N/A
N/A
351
319
158
ND
484
90
392
N/A
113
232
17
N/A
N/A
635
60
415
N/A
N/A
209
122
284
N/A
862
45
474
N/A
N/A
163
109
738
ND
388
90
367
N/A
N/A
286
ND
674
N/A
TABLE 32B
TOTAL PCB IN CONDENSATE
(ng/L)
Run Number A2 A3 Bl B2 Cl C2 C3 Dl
1 1 1 1 1 II
SAMPLE POINTS * 1 1 1 1 1 II
1 1 1 1 1 II
Liq. from 1st Condenser (9L) | 246981 27343 | N/A | ND | 25956 392691 5814| ND
I 1 1 1 1 II
III!! II
Liq. from 2nd Condenser (10L)| 661861 69074 | 27605 | ND | 12692 178901 19471 | ND
1 1 1 1 1 II
N/A - Not Analyzed
ND - None Detected
* Process conditions same as for sediment
Highlighted values are averages of multiple (3-5) measurements.
DATA SOURCE: Referenced Battelle Report
81
-------
TABLE 33
SUMMARY OF CALCULATIONS
PCB IN SOLIDS
< MG OUT >
PERCENT
BIN
A2
A3
Bl
B2
Cl
C2
C3
Dl
MG
IN
ND
ND
63.
189.
90.
91.
69.
87.
5
2
0
8
3
8
RESIDUE
ND
ND
35
267
6
52
44
0
.3
.3
.7
.8
.8
CONDENSATE REMOVED
ND
ND
1.
0.
4
2
N/A
0.
2.
1.
6
6
1
44
0
92
42
35
100
.4
.0
.6
.5
.4
.0
3.1.8 Solidification/Stabilization of Treated Residue
Following application of the RETEC thermal desorption
technology, the U.S. Army Corps of Engineers solidified selected
batches of treated sediment residue with cement. The intent of
this action was to curtail mobility of the pollutants remaining
in the residue. Four distinct ratios of cement-to-residue ratios
were employed: 0.1, 0.2, 0.4, and 0.6. Solidified residues were
cured for approximately one month and then tested to determine
unconfined compressive strength and degree of pollutant
attenuation for Cr, Cu, Hg, Pb, and TOC as measured'by either the
toxicity characteristic leach procedure (TCLP) or the sequential
batch leach test (SBLT). (TCLP is performed in a single leach
step while SBLT is performed using 4 sequential extractions.)
Results of this work appear in Tables 34 through 36.
From these tests it is concluded that unconfined compressive
strength varied directly as cement: residue ratio, indeed the
correlation coefficient relating the two variables was 0.994.
Additionally, assessments of results for TCLP and SBLT follow:
TCLP:
Because treated, unsolidified sediment contained no
mercury, it was not possible to determine whether solidification
could attenuate the mobility of mercury.
Solidification of the treated residue resulted in an 89
percent reduction in extract Pb concentration. Reduction was not
correlated with cement: residue ratio.
82
-------
TABLE 34
SOLIDIFICATION/STABILIZATION UNCONFINED
COMPRESSIVE STRENGTH (UCS) RESULTS
Run
No.
B1-B3
B1-B3
B1-B3
A2
A2
A2
A2
A3
A3
A3
A3
B2
B2
B2
Cement to -
Residue Ratio
0.1
0.1
0.1
0.2
0.2
0.2
0.2
0.4
0.4
0.4
0.4
0.6
0.6
0.6
USC Average Std. Dev. Coefficient of
(Ibs/sq in.) Clbs/sq in.) (Ibs/sq in.) Variation (Percent)
208
203 250 77 30.7
338
433
410 388 48 12.3
323
384
925
836 898 59 6.6
968
865
1277
1115 1212 86 7.1
1245
DATA SOURCE: Corps of Engineers Waterways Experiment Station
TABLE 35
RESULTS OF RESIDUE STABILIZATION
CONCENTRATIONS OF EXTRACTS FROM
TOXICITY CHARACTERISTIC LEACH PROCEDURE (TCLP)
BIN
CEMENT TO
RESIDUE RATIO
CONCENTRATION IN ug/L
Cr Cu Hg Pb
UCS
BEFORE
STABILIZATION
AFTER
STABILIZATION
A2
A3
B2
B1/B3
A2
A3
B2
B1/B3
0
0
0
0
.2
.4
.6
.1
0.
0.
0.
0.
36
44
17
2
27
71
13
69
.5
.4
.9
.0
4
15
2
13
42
12
13
30
.2
.1
.4
.6
.3
.0
.1
.8
ND
ND
ND
ND
ND
ND
ND
.008
2.57
6.55
1.93
6.16
ND
ND
.72
1.07
388
898
1212
250
f^=
6.21
6.10
6.23
6.10
10.94
11.67
12.06
6.61
DATA SOURCE: Referenced Battelle Report
83
-------
TABLE 36
SEQUENTIAL BATCH LEACH TEST (SBLT) FOR METALS
CEMENT TO
RESIDUE
BIN RATIO
BEFORE
STABILIZATION
AFTER
STABILIZATION
CHANGE
A2
A3
B2
B1/B3
A2
A3
B2
B1/B3
A2
A3
B2
B1/BC
0.2
0.4
0.6
0.1
0.2
0.4
0.6
0.1
CR
Avg. Value
1st FR.
0.4
1.0
ND
0.6
8.4
12.2
11.8
6.1
+8.0
+11.2
+11.8
+5.5
(ug/L)
Avg. Value
£ FR. 2-4
0.8
0.7
ND
1.9
22.4
34.9
44.7
12.1
+21.6
+34.2
+44.7
+10.2
Cu (uq/L)
Avg. Value Avg. Value
1st FR T. FR. 2-4
1.1
20.1
2.4
4.7
60.2
15.1
16.9
125.4
+59.1
-5.0
+14.5
+120.7
5.2
8.7
ND
10.4
83.7
17.3
24.5
234.2
+78.5
+8.6
+24.5
+223.8
Hg (ug/L)
Avg. Value
1st FR
ND
0.00149
0.0047
0.00054
0.00101
0.00030
0.00026
0.00104
+0.00101
-0.00419
-0.00021
+0.00050
Avg. Value
2 FR 2-4
0.00101
0.00356
ND
0.00320
0.00204
0.00126
0.00094
ND
+0.00103
-0.00230
+0.00094
-0.00320
Pb (ug/L)
Avg. Value
1st FR
ND
ND
ND
ND
8.1
7.1
6.8
13.4
8.1
7.1
6.8
13.4
Avg. Value
Z FR 2-4
3.4
9.3
ND
7.2
11.0
15.1
16.7
8.2
+7.6
+5.8
+16.7
+1.0
DATA SOURCE: Referenced Battelle Report
-------
Leachability of Cu and Cr were increased by
solidification. Leachability is not correlated with cement:
residue ratio, thus the cause of increased Cu and Cr leaching in
solidified material is unknown.
SBLT:
Attenuation of TOG mobility in solidified residue is
variable, as measured by Steps 1-4 of the SBLT leach test. These
results are shown graphically in Figure 17. In two cases
mobility was attenuated and in two cases it was enhanced. These
results do not correlate with cement: residue ratio, thus the
reason for this pattern is unknown.
Mobility of all metals but mercury was generally enhanced
by the stabilization procedure. Mercury results were variable.
3.2 FULL SCALE IMPLEMENTATION
The following discussion provides a description and cost
estimate for a full scale remediation of contaminated sediments
using the thermal desorption process. Two separate cost
estimates were made for sediment remediation involving 10,000 and
100,000 cubic yards of material. These quantities were believed
to represent feasible cleanup scenarios for areas with heavily
polluted sediments. Due to the anticipated high cost per cubic
yard of such a cleanup it did not seem reasonable that millions
of cubic yards or several 100's of thousands of cubic yards would
be remediated using the thermal desorption process.
3.2.1 Thermal Desorption Remediation
The following discussion provides a description of the
thermal desorption system and a cost estimate for the remediation
of 10,000 and 100,000 cubic yards of contaminated sediments. In
preparing the estimates for sediment treatment, it was assumed
that all processing would be conducted at a centralized facility
on-site and that the moisture content of the sediments would be
adjusted to approximately 60 percent by weight to facilitate
handling and treatment operations.
The application of the thermal desorption technology
provides for the volalitized components to be condensed and
separated into concentrated streams. The aqueous condensate
would be treated on-site and combined with the treated solids for
dust control, while the concentrated organic condensate would be
transported off-site for disposal in a permitted facility.
3.2.1.1 Full-Scale Treatment System—
A nominal processing rate of approximately 41 tons per day
(34 cubic yards at 1.2 tons per yard) was assumed. The
processing system would have a rated capacity of 2.0 tons per
hour for a three shift-per-day operation. A system utilization
rate of 85 percent was assumed to provide time for routine
maintenance and repair. The proposed throughput assumes a solids
residence time of 120 minutes for the full-scale remediation
based on the results of the pilot scale demonstration which
85
-------
FIGURE 17
RESULTS OF RESIDUE STABILIZATION: TOC ANALYSIS
OF EXTRACTS FROM SEQUENTIAL BATCH LEACH TEST (SBLT)
FIGURE 17A: BIN A2 CEMENT: RESIDUE RATIO = 0.2
100
(12.0)
o
o
o
50 -
(7.6)
(7.8)
F1 F2 F3 F4
BEFORE TREATMENT
F1 F2 F3 F4
AFTER TREATMENT
FIGURE 17B: BIN A3 CEMENT: RESIDUE RATIO = 0.4
150
(7.4)
100
o
o
o
50
F1 F2 F3 F4
BEFORE TREATMENT
11.0)
F1 F2 F3 F4
AFTER TREATMENT
F# = FRACTION NUMBER
NUMBER IN PARENTHESIS IS PH OF ASSOCIATED LEACHATE
86
-------
FIGURE 17C: BIN B2 CEMENT: RESIDUE RATIO = 0.6
100 r-
\
o
o
o
50
(7.3)
(7.7
F1 F2 F3 F4
BEFORE TREATMENT
(12.3)
12.5)
(12.4)
12.3)
F1 F2 F3 F4
AFTER TREATMENT
FIGURE 17D: BIN B1/B3 CEMENT: RESIDUE RATIO = 0.1
(7,3)
150 i-
x
o
O
O
100
50
(7.5)
(7.7)
//A
(7.
F1 F2 F3 FA
BEFORE TREATMENT
112.3)
(12.2)
(12.1 )
(12.0)
F1 F2 F3 F4
AFTER TREATMENT
F*t = FRACTION NUMBER
NUMBER IN PARENTHESIS IS PH OF ASSOCIATED LEACHATE
87
-------
indicated that the extended residence would be required to
ensure the removal of organic contaminants.
Material Feed - The moisture content of the dredged
material would be adjusted to approximately 60 percent prior to
screening and treatment. The addition of water and associated
mixing would be conducted on a semi-continuous basis. Agitation
of the material would be conducted using propeller agitator
mixers. Aqueous condensate from the process would be used for
make-up water. The sediments would then be pumped from the tanks
to the processor at a flow consistent with the proposed
processing rate, approximately 6 gallons per minute. The inlet
pump line and the pump effluent would be screened to exclude
over-sized material or debris. Accumulated oversized material
would be removed from the bottom of the tanks during routine
maintenance. A positive displacement-style pump would be
utilized in transferring the sediments from the tank to the
treatment unit.
Thermal Processor - The initial processor in the system
is designed to remove moisture and organics from the feed
material and reduce the volume of the material for subsequent
disposal. A model D-24-24 screw dryer manufactured by the Denver
Equipment Company, with a capacity of 2.0 tons per hour, would be
used in the processor. The Denver processor uses a contained,
non-contact circulating heat transfer fluid to raise the
temperature of the solids being treated. Based on results of the
pilot scale demonstration, it was assumed that final solids
temperatures of 600 to 700° F would be required to ensure the
complete removal of organics. The heat transfer fluid for the
full scale remediation would be COASTAL HI-TEC salt, which has a
maximum operating temperature of 1,100° F. The heat transfer
media would be heated with an oil fired system having a capacity
to circulate fluid at a rate of 200 gallons per minute (gpm) and
provide approximately 3.0 million BTU/per hour to the processor
(Remediation Technologies, Inc., 1992).
The final component of the system would be designed to cool the
solids to a temperature of 140° F for subsequent handling. The
cooling screw would require approximately 20 gpm of cooling
water.
It is believed that the build up of feed material around the
thermal processor augers could be prevented during a full scale
operation by maintaining a feed moisture content of approximately
60 percent. If it were found that the caking of material
persisted, the Holo-Flite Screw Processor System could be
replaced with a system that continuously self cleans the internal
surfaces of the processor.
The off-gas handling system would consist of a cylone, quench
chamber, indirectly-cooled condenser and activated carbon beds.
The off gas control system would be designed to accommodate an
off-gas flow rate of approximately 2500 cubic feet per minute at
600° F, and "worst case" moisture and organic loading of 2400
pounds per hour and 4 pounds per hour respectively. A cyclone
particulate removal system would remove any fine solid
particles (>10 urn) which may be entrained with the off-gases.
88
-------
These solids would be removed and combined with the feed material
for reprocessing. The volatilized organics and moisture would be
condensed into a combined liquid stream. The condenser would be
designed to achieve 90 percent removal of organics and moisture
in the gas. Separation of the organics and aqueous condensate
streams would be enhanced by the use of a coalescing plate
separator. The condensed organics would be disposed of off site.
Approximately 5 gpm of aqueous condensate would be generated
as a result of treatment operations. One half of the condensate
would be used to dilute the dredged sediments in the mixing
tanks, while the remaining volume of condensed water would be
treated on site using biological treatment or activated carbon.
After the liquid and particulate are removed from the purge gas
stream the gas would be treated to remove residual volatile
organics. Treatment would consist of filtration through
granulated activated carbon beds.
3.2.1.2 Cost Estimate for Sediment Remediation—
Cost estimates for the remediation of 10,000 and 100,000
cubic yards of contaminated sediment using the thermal desorption
technology were prepared. The estimated operating costs (+/- 20
percent) for treating the contaminated sediments on site are
shown in Tables 36 and 37. Unit prices were determined using a
processing rate of 890 tons (612 cubic yards of "as-dredged"
material (40 percent moisture) per month, assuming a 24 hour per
day operation with an 85 percent system utilization rate. The
estimate includes costs for all mobilization/demobilization,
thermal treatment, associated analytical activities, on-site
treatment of the aqueous condensate, and the off-site disposal of
the organic condensate stream. Costs associated with sediment
excavation and transport to the treatment site were not included.
These costs can be expected to be less than 10 percent of the
associated remediation cost discussed below. Engineering and
design work would add approximately 10 percent to the project
cost, as would construction management. Therefore, total project
cost would be roughly 1-1/3 times the remediation cost shown
below.
Remediation of 10,000 Cubic Yards - Treatment costs for
processing this volume of waste were estimated at $535 per cubic
yard, with the work being completed in approximately 16 months.
Mobilization and demobilization costs were estimated to be
$500,000 while the monthly equipment charge was estimated at
$132,000. The equipment charge was calculated to provide a 25
percent return on capital investment over the duration of the
contract.
Field labor and utilities were estimated to make up approximately
30 percent of the total treatment cost. The labor costs includes
4 workers per shift and three shifts per day at an average hourly
rate of $35, including overhead. Utility costs are based upon
the fuel requirements to maintain the temperature of the heat
transfer media during treatment, and the electrical requirements
of the system (200 kw, 480 v, 225 amp).
Maintenance and activated carbon disposal comprise less than 5
percent of the cost. Activated carbon disposal/replacement was
estimated at $1000 per month. Carbon would be recharged and
89
-------
reused until its useful life was exhausted. Spent carbon would
be disposed of by landfilling or incineration if required. The
off-site disposal of the condensated liquid organics was
conservatively estimated at $1000 per ton while the on-site
treatment of the aqueous condensate was estimated to cost $0.02
per gallon. This cost equates to approximately $8 per ton of
dredged sediment. The total cost for processing 10,000 cubic
yards of sediments was estimated at $5,350,000 and is shown in
Table 37.
Remediation of 100,000 Cubic Yards - The cost estimate
for treating 100,000 yards of contaminated sediments includes the
use of four parallel treatment systems to allow the completion of
the remediation in a reasonable time period. As discussed
previously, each system would process 612 cubic yards of "as-
dredged" sediments per month, assuming a 24 hour per day
operation with an 85 percent system utilization rate. With this
treatment train, the sediment remediation work could be completed
within 41 months at an estimated unit cost of $352 per cubic
yard. Mobilization and demobilization costs were estimated to be
$1,200,000, or $12 per cubic yard of sediment. Other operating
expenses such as fuel, maintenance and waste disposal will have
unit costs similar to those discussed under the smaller treatment
scenario.
Monthly equipment charges for the four treatment units were
estimated to be $363,000, resulting in a monthly charge per
individual unit that is significantly less than the monthly
charge for the single unit anticipated for the remediation of
10,000 cubic yards of sediment. This is due to the increased
period of time, 41 verses 16 months, available to recover the
capital investment. The total cost for processing 100,000 cubic
yards of contaminated sediments was estimated to be $35,200,000
and is shown in Table 38.
Variations in the moisture content can impact the thermal
requirements, while variations in the organic content of the feed
sediment would primarily affect the pricing of services by
changing the rate of activated carbon usage. RETEC does not
believe that any of these factors or material processing
requirements would significantly affect the throughput of the
system or the estimated cost of treatment (Remediation
Technologies, Inc., 1992).
3.3 CONCLUSIONS AND RECOMMENDATIONS
3.3.1 Conclusions
A review of the results from the program provides the
following conclusions related to material composition, material
handling, effectiveness of treatment, and process operation.
1. Material Handling - The dredged materials were
relatively free of debris or over-sized material which would
adversely affect the processing of the sediments during full-
scale implementation. Some problems were caused by the physical
90
-------
TABLE 37
COST ESTIMATE FOR REMEDIATING 10,000 CUBIC YARDS OF SEDIMENT
DESCRIPTION ESTIMATED COST
Mobilization and Demobilization (Treatment) $ 500,000
Equipment Rental 2,150,000
Utilities: Fuel 250,000
Electricity: Cooling 320,000
Misc. 160,000
Operating Field Labor 1,630,000
Maintenance 80,000
Activated Carbon 20,000
Other Operating Costs 160,000
Disposal of Organic Condensate
and Treatment of Aqueous Condensate 80,000
TOTAL $5,350,000
TOTAL COST PER CUBIC YARD $ 535
DATA SOURCE: Referenced RETEC, Inc. Report
TABLE 38
COST ESTIMATE FOR REMEDIATING 100,000 CUBIC YARDS OF SEDIMENT
DESCRIPTION ESTIMATED COST
Mobilization and Demobilization $ 1,200,000
Equipment Rental 14,900,000
Utilities: Fuel 2,500,000
Electricity: Cooling 3,200,000
Misc. 1,000,000
Operating Field Labor 9,600,000
Maintenance 800,000
Activated Carbon 200,000
Other Operating Costs 1,000,000
Disposal of Organic Condensate
and Treatment of Aqueous Condensate 800,000
TOTAL $35,200,000
TOTAL COST PER CUBIC YARD $352
DATA SOURCE: Referenced RETEC, Inc. Report and Corps of
Engineers, Buffalo District
91
-------
characteristics of the material: (1) Sediments can cause
conveyance problems for solids handling systems such as
conveyors, bucket elevators, and screw conveyors due to their
cohesive properties. However, the feed material was determined
to be readily pumpable at moisture contents above 45 percent by
weight. (2) Dried sediments can collect in the processor,
eventually preventing the rotation of the screw auger. Results
from the pilot scale demonstration indicate that this problem was
more pronounced when feed material with lower moisture contents
were being processed. Minimal problems were encountered when
processing material with a moisture content in excess of 50
percent by weight. From the limited data available it was not
clear if this was due to a physical change in the properties of
the solids or is the result of a lower mass feed rate of solids
due to dilution with water.
2. Process Operations - After initial optimization of the
material handling system, the technology operated without
significant problems and provided the following information. In
general, the heat transfer characteristics for the sediment were
low, resulting in exit solids temperatures that were
significantly lower than anticipated, 300 to 535°F versus 700°F.
Residence times of 60 minutes were appropriate to achieve
moisture removal/mass reduction, while consistent organic removal
required treatment for periods in excess of 90 minutes.
Particulate buildup in the off-gas control system was not a
significant problem due to the high moisture content of the feed
material. One of the operating results was the poor separation
of the organic and aqueous condensates due to the dilute nature
of the oil stream. RETEC attempted to separate the streams by
"controlled condensation," separation on the basis of
condensation temperature. This proved to be largely
unsuccessful, probably due to the low concentration of organics
versus moisture in the waste. Results from several test runs
indicated that the aqueous and organic streams generally
contained low concentrations of volatile organics which were
concentrated to some degree in the organic stream. Effective
separation of such a dilute stream would require the use of a
physical separator.
3. Feed material containing 44-56 percent solids was
successfully pumped and dryed to a solids content > 95 percent.
4. Removal levels for constituents of concern were
contaminant specific. Ranges of removal for each constituent of
concern were as follows:
a. Mercury: 9-100%
b. Low molecular weight polycyclic aromatic
hydrocarbons: 45-90%
c. High molecular weight polycyclic aromatic
hydrocarbons: 42-96%
d. Oil and grease: 17-86%
e. Total organic carbon (TOC): 5-35%
92
-------
f. Polychlorinated biphenyls (PCBs): 0-100%
g. Chromium: 0-9%
h. Copper: 0-11%
i. Lead: 0-13%
5. Removal of organic materials was not strongly correlated
with measured process conditions such as maximum sediment
temperature, residence time, and percent moisture in the feed.
Some other parameter is controlling removal.
6. Since copper, chromium, and lead remain with the treated
sediment, the dryed sediment is a potential candidate for
remediation by a stabilization/solidification technology. While
stabilization/solidification with a cementitious process was not
successful for chromium and copper when the material was ground
up, it is possible that chromium and copper leachability would be
negligible if the unground material was tested by exposure to
normal weathering processes.
7. Solvent extractables and "TOC" are both potentially
usable as surrogate parameters for predicting removal of high
molecular weight PAHs.
8. Air emissions were measured for PAHs, dioxins, furans,
and PCBs, and were extremely low:
Low molecular weight PAHs: 1.6 - 18.0 mg/hour
High molecular weight PAHs: 0.4 - 8.6 mg/hour
Dioxins: 0.005 - 0.017 mg/hour
Furans: 0.000 - 0.032 mg/hour
PCBs: 1.3 - 2.4 mg/hour
9. It is of interest to determine the percent of each
hazardous material entering the processor that was released to
the atmosphere via air emissions. This value was quantifiable
for PAHs only; < 0.004 percent of the PAHs in the feed material
were discharged via air emissions.
10. Stabilization/solidification of the treated residue
resulted in an 89 percent attenuation of the mobility of lead.
Leachability of copper and chromium were increased.
11. Fate of the removed materials was not determined in
many cases. Factors contributing to this problem were (1) the
combining of stream rates rather than taking individual weights,
(2) slight particulate losses at the processor seals, (3)
processing of relatively clean sediment, (4) exclusion of metals
analysis in the air sampling, and (5) failure to quantify
materials captured by carbon.
3.3.2 Recommendations/Lessons Learned
The following recommendations are made for performing future
pilot studies in thermal desorption.
1. Operation at higher temperatures should be considered to
93
-------
assess whether higher removal levels can be achieved for semi-
volatiles and other organic materials.
2. Individual weights of each stream should be obtained
rather than combined weights (e.g., Solids from each cyclone
should be weighed and recorded, as should the treated residue.
The solids should not all be combined and then reported as a
single weight.). The taking of individual weights will make it
possible to determine the fate of each contaminant.
3. Analysis of air emissions should include analysis for
metals.
4. Sediments with greater contaminant levels should be
selected for treatment. A large percent error is inherent in
measurements and mass balances for low concentrations of
contaminants.
5. Use of solvent extractables and/or "Total Organic
Carbon" as surrogate parameters for estimating removal of high
molecular weight PAHs should be further investigated.
6. Analysis of activated carbon for organics and metals
should be considered and carried out. PAHs and PCBs are likely
partitioning to the carbon in the emissions system, because of
the fundamental nature of activated carbon to adsorb organics.
3.3.3 The following recommendations concern the use of the
thermal desorption and solidification for sediment remediation:
1. Thermal desorption should be tried again at higher
temperatures/longer residence times to achieve a more complete
assessment of organic contaminant removal ability is made.
2. Thermal desorption should be applied to a more
contaminated feed material than the Buffalo River sediments
before an assessment of organic contaminant removal ability is
made.
3. Solidification/stabilization is not practical for Buffalo
River residues, as two of the three metal contaminants (Cu, Cr)
leach more quickly when solidified than when the material has not
been treated in this way.
94
-------
REFERENCES
Aqua Tech Environmental Consultants. The Analyses of Sediments
from Buffalo Harbor and Sediment Analyses, Buffalo River and
Harbor, Buffalo, NY. Aqua Tech Environmental Consultants,
Inc., Melmore, Ohio, 1989.
Averett, Daniel E.. Strategy for Selection of Sites and
Technologies for Pilot-Scale Demonstration Projects, Draft
Paper, U.S. Army Engineer Waterways Experiment Station,
Vicksburg, MS, 1990a.
Averett, Daniel E., Perry, Brett D., Torrey, Elizabeth J., and
Miller, Jan A. Review of Removal, Containment, and
Treatment Technologies for Remediation of Contaminated
Sediment in the Great Lakes. Miscellaneous Paper EL-90-25,
US Army Engineer Waterway Experiment Station. Vicksburg,
MS, 1990b.
Battelle Marine Research Laboratory. Report of Chemical Analyses,
Buffalo River Pilot Project, Volumes 1-3, Battelle Marine
Research Laboratory, Sequim, Washington, 1992.
Department of the Army. Dredging and Dredged Material Disposal.
Engineering Manual EM 1110-2-5025, Department of the Army,
U.S. Army Corps of Engineers, Washington, DC, 1983.
E-Three, Inc. Stack Emission Test Report, Demonstration Thermal
Desorption Project, Buffalo River Sediments. E-Three, Inc.,
Buffalo, NY, 1992.
Fleming, Elizabeth C., Averett, Daniel E., Channell, Michael G.,
and Perry, Bret D. An Evaluation of Solidification/
Stabilization Technology for Buffalo River Sediment.
Miscellaneous Paper EL-91-11, US Army Engineer Waterways
Experiment Station, Vicksburg, MS, 1991.
New York State D.E.C. Buffalo River Remedial Action Plan, New
York State Department of Environmental Conservation, Albany,
New York, 1989.
New York State D.E.C. Buffalo River Remedial Action Plan Annual
Report. New York State Department of Environmental
Conservation, Albany, New York, 1992.
Remediation Technologies, Inc. Field Demonstration of RETEC
Thermal Unit for Remediation of Buffalo River Sediments,
Buffalo River Area of Concern, Remediation Technologies,
Inc., Concord, Massachusetts, 1992.
-------
U.S. Array Engineer District, Buffalo. Buffalo River
Demonstration Dredging Project, Buffalo Harbor, Erie County,
New York; Finding of No Significant Impact/Environmental
Assessment. U.S. Army Engineer District, Buffalo, New York,
1992.
U.S. Army Engineer Waterways Experiment Station. Quality
Assurance Project Plan; Buffalo River Pilot Demonstration of
Low Temperature Thermal Desorption for Treating Contaminated
Sediments. U.S. Army Engineer Waterways Experiment Station,
Vicksburg, MS, 1991.
U.S. Environmental Protection Agency. Assessment and Remediation
of Contaminated Sediments (ARCS) Work Plan, U.S.
Environmental Protection Agency. Great Lakes National
Program Office, Chicago, Illinois, 1990.
Verschueren, K., Handbook of Environmental Data on Organic
Chemicals, Van Nostrand Reinhold, New York, 1983.
-------
APPENDIX A
SAMPLE CALCULATIONS
-------
SAMPLE MASS BALANCE CALCULATION
MASS BALANCE FOR CHROMIUM
PART A: ADJUSTMENT OF STREAM WEIGHTS TO DRY WEIGHT BASIS:
Al: NO DATA
A2:
INPUT
(2010 Ibs) X (.554 Ibs drv solids') x (.454 kg) = 505 kg dry solids
Ib Ib
OUTPUT SOLIDS
Average % solids in treated solids + cyclone residue =
(1055 Ib) x (.998) x (0.454) = 478 kg
OUTPUT LIQUIDS
(890 Ib) x (.011 Ib solids/lb liquid) x (0.454) = 4.4 kg
A3:
INPUT (2150)(.550)(.454) = 537 kg
OUTPUT SOLIDS (1235)(. 995)(.454) = 557 kg
OUTPUT LIQUIDS (688)(.008)(.454) = 2.5 kg
Bl
INPUT (1355)(.561)(.454) = 345
OUTPUT SOLIDS (845)(.986)(.454) = 378
OUTPUT LIQUIDS (620)(.008)( .454) =2.3
B2
INPUT (2175)(.546)(.454) = 539 kg
OUTPUT SOLIDS (1850)(.998)(.454) = 838 kg
OUTPUT LIQUIDS (445)(.007)(.454) = 1.4 kg
A-l
-------
Cl
INPUT (1640)(.521)(.454) = 388
OUTPUT SOLIDS (880)(.998)(.454) = 398
OUTPUT LIQUIDS (840)(.009)(.454) =3.4
C2
INPUT (1905)(.508)(.454) = 439
OUTPUT SOLIDS (955)(.999)(.454) = 433
OUTPUT LIQUIDS (880)(.005)(.454) = 2 kg
C3
INPUT (1940)(.483)(.454) = 425
OUTPUT SOLIDS (950)(. 952)(.454) = 411
OUTPUT LIQUIDS (850)(.009)(.454) = 3.5
Dl
INPUT (1515)(.446)(.454) = 307
OUTPUT SOLIDS (700)(.999)(.454) = 317
OUTPUT LIQUIDS (950)(.004)(.454) =1.7
SOLIDS BALANCE
RUN SOLIDS INPUT SOLIDS OUTPUT SOLIDS OUTPUT IN LIQUID
(kg) (kg) (kg)
4.4
2.5
2.3
1.4
3.4
2.0
3.5
1.7
For numbers in parentheses, output exceeds input according to calculations.
Possible reasons include material holdup in the equipment and errors inherent
in the analytical test methods.
A-2
A2
A3
Bl
B2
Cl
C2
C3
Dl
505
537
345
539
388
439
425
307
478
(557)
(378)
(838)
(398)
433
411
(317)
-------
MASS BALANCES/METALS
Chromium
(A2)
505,000 g solids (47xlO'6 g Cr) = 23.7 Cr in
g solids
Since it is not known what % of total solids came from the cyclones, the
following is assumed for these calculations:
cyclone 1: 4%
cyclone 2: negligible
.'. Overall concentration of processed solids is:
.96(70) + .04(137) = 73 ug/g
IN SOLIDS:
(477,000 g) x (73 x 10'6 g Cr) = 34.8 g
g
IN CONDENSATE SOLIDS: Consider this negligible
(4,400 g) (137 x 10'6 g) = .60 g
In Condensate:
890 Ibs (.454 kg) = 404 kg - 4 kg solids output from liquid
Ib
404 kg L (13.130 x 10'6 g Cr - 5.2 grams
kg L
A3: In: (537,000)(68)(10"6) = 36.5 Cr in
.96(61) + .04(148) « 65 ug/g
Out: (557,000)(65xlO"6) = 36.2 Cr in treated solids
Out/Liquids: Correction to liquid amount by removing amount solids is
negligible and is ignored for this and future calculations.
(688U454)(14.2QQ x 1Q'6) = 4.4 g
(1000)
A-3
-------
In: (345,000)(47)(10~6) - 16.2 g
(0.96)(56) + (0.04X129) ~ 59 ug/g
Out (solids): (378,000)(59 x 10~6) = 22.3 g
Out (liquid): (620) (454X1847 x 10'6) = 0.5 g
(1000)
B2: In: (539,000)(58)(10"6) = 31.3 g
0.96(44) + 0.04(106) » 47 ug/g
Out (solid): (838,000)(47)(10"6) - 39.4 g
Out (liquid): (445)(454)(200)(10'6) = 0.04 » 0 g
(1,000)
B3: Closure too poor to consider mass balance on Cr.
£1: In: (388,000)(73)(10'6) = 28.3 g Cr in
0.96(67) + 0.04(136) = 70 ug/g Cr in treated solids
(398,000)(70xlO~6) - 27.9 g
Out (liquid): (840)(454)(830)(IP'6) = 0.3 g
1000
C_2: In: (439,000(59) (10"6) = 25.9 Cr in
.96(58) + .04(129) « 61 ug/g Cr
Out: (433,000(61)(10"6) = 26.4 Cr in treated solids
Out (liquid): (880)(454)(410)(10'6) = 0.2 g Cr
1000
A-4
-------
C3: In: (425,000)(69)(10'6) = 29.3 Cr in
0.96(62) + 0.04(140) = 65 ug/g
Out: (411,000)(65)(10~6) = 12.1 g Cr out with solids
Out (Liquid): (454H850U114QU10'6') = 0.4 g Cr
(1000)
Dl: In: (307,000)(55)(10"6) = 16.9 g Cr
0.96(62) + 0.04(112) = 64 ug/g
Out: (317,000)(64)(10~6) = 20.3 g Cr in solids
Out (liquid): (950) (454) (723U 10'6) =0.3
1000
A-5
-------
CORRELATION COEFFICIENT:
r - (5 (Xi - x) (Yi - y)/[(Xi - x)2(Yi - y)2]172
WHERE: x^ = given value of process variable (e.g., temperature)
y£ = given value of measured parameter (e.g., % solids)
x = average value of process variable
y = average value of measured parameter
A-6
-------
AIR EMISSIONS OF POLYCHLORINATED BIPHENYLS
PCB
Minimum
LBS/Hour Grams/Hour
Maximum
LBS/Hour _Grams/Hour
Monochlorobiphenyl
Dichlorobiphenyl
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobiphenyl
Octachlorobiphenyl
Nonachlorobiphenyl
Decachlorobiphenyl
TOTAL
1.25E-07
1.25E-07
1.25E-07
2.49E-07
2.49E-07
2.49E-07
3.82E-07
3.82E-07
3.82E-07
6.31E-07
2.90E-06
5.67E-05
5.67E-05
5.67E-05
1.13E-04
1.13E-04
1.13E-04
1.73E-04
1.73E-04
1.73E-04
2.86E-04
1.32E-03
2.23E-07
2.23E-07
2.23E-07
4.46E-07
4.46E-07
4.46E-07
6.84E-07
6.84E-07
6.84E-07
1.13E-06
5.19E-06
1.01E-04
1.01E-04
1.01E-04
2.02E-04
2.02E-04
2.02E-04
3.11E-04
3.11E-04
3.1 IE -04
5.13E-04
2.23E-03
AIR EMISSIONS OF PARTICULATES
Minimum
LBS/Hour Grams/Hour
Maximum
LBS/Hour Grams/Hour
Particulates
0.0019
0.086
0.0026
1.18
A-7
-------
AIR EMISSIONS OF POLYCYCLIC AROMATIC HYDROCARBONS
Minimum
Maximum
PAH
Naphtahalene
Acenapthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benz (a) anthracene
Chrysene
Benzo ( b j k) f luo ranthrene
Benzo(a)pyrene
Indo(l ,2,3- cd)pyrene
Dibenz(a , h) anthracene
Benzo (g ,h, i)perylene
2
3
9
1
9
1
3
2
4
5
9
2
1
1
2
.35E
.01E
.65E
. 16E
.58E
.04E
.89E
.22E
.38E
.30E
.52E
.63E
.99E
.90E
.70E
-06
-08
-08
-08
-07
-07
-07
-07
-08
-08
-08
-08
-08
-08
-08
1
1
4
5
4
4
1
1
1
1
2
4
1
9
8
1
405
.07E-03
.37E-05
.38E-05
.27E-06
.35E-05
.72E-05
.22E-03
.77E-04
.OOE-04
.99E-05
.40E-05
.32E-05
.19E-05
.03E-06
.63E-06
.22E-05
.86E-06
2
1
2
1
7
9
2
4
9
1
4
5
1
1
5
.58E
.26E
.49E
.14E
.92E
.51E
.33E
.56E
.16E
.04E
.72E
.1.6E
.28E
.22E
.46E
-05
-06
-06
-06
-06
-06
-06
-06
-06
-06
-07
-07
-07
-07
-07
1
5
1
5
3
4
2
1
2
4
4
2
2
5
5
2
857
. 17E
.72E
.13E
. 18E
.60E
,32E
. 18E
.06E
.07E
. 16E
.72E
. 14E
.34E
.81E
.54E
,48E
. 15E
-02
-04
-03
-04
-03
-03
-02
-03
-03
-03
-04
-04
-04
-05
-05
-04
-05
TOTAL
4.44E-06
2.02E-03
5.86E-05 2.66E-02
DIOXIN
AIR EMISSIONS OF DIOXINS*
Minimum Maximum
nanograms/sec nanograms/hour nanograms/sec nanograms/hour
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
TOTAL
7
3
8
5
6
1
1
.OOE
.46E
.67E
.33E
.67E
.67E
.30E
-04
-04
-05
-05
-05
-05
-05
2
1
0
0
0
0
.52
.25
.31
.19
.24
.06
0.04
4
.61
1
2
2
2
2
2
8
.66E
.01E
.68E
.41E
.72E
.91E
-03
-03
-04
-04
-04
-04
.99E-05
5
7
0
0
0
1
.98
.24
.96
.87
.98
.05
0.32
17
.40
* Emissions reported as 2378-TCDD Toxicity Equivalents (EPA 1989)
A-8
-------
FURAN
AIR EMISSIONS OF FURANS*
Minimum Maximum
nanograms/sec nanograms/hour nanograms/sec nanoerams/hour
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678 -HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
O.OOE+00
O.OOE+00
O.OOE+00
O.OOE+00
1.47E-05
O.OOE+00
O.OOE+00
O.OOE+00
O.OOE+00
O.OOE+00
0.00
0.00
0.00
0.00
0.05
0.00
0.00
0.00
0.00
0.00
6.08E-05
O.OOE+00
5.48E-03
1.30E-03
1.07E-03
7.12E-05
3.38E-04
3.68E-04
O.OOE+00
O.OOE+00
0.22
0.00
19.73
4.68
3.85
0.26
1.22
1.32
0.00
0.00
TOTAL
0.05
32.28
Emissions reported as 2378-TCDD Toxicity Equivalents (EPA 1989)
A-9
-------
APPENDIX B
UNREDUCED ANALYTICAL DATA
-------
REPORT OF CHEMICAL ANALYSES
Volume I: Metals and Conventionals
PROJECT: Buffalo River Pilot Project
Prepared for:
USEPA Great Lakes National Program Office
Attn: Dr. Steve Garbaciak
230 S. Dearborn
Chicago. IL 60604
-------
SAMPLE LABEL KEY
Sample label key is explained by using the following examples:
070CT 12:34 JLS A O *- Label
(1) (2) (3) (4) (5) «- Key
(1) Date of sample
(2) Time of sample
(3) Sampling point number from Figure 10
Where S = solid stream
L = liquid stream
G = gas stream
(4) Bin (A,B,C, or D: There were 4 bins filled)
(5) Type of sample, where:
O = organic
M = metal
L = leach test
G = grain size
S = solids
C = Total Organic Carbon (TOC)
When sample has additional number preceding the last letter of
the series, i.e.
230CT 4:28 4S A2. O
The number is a run number, i.e. Run 2 from Bin A
-------
REPORT OF:
PROJECT:
ISSUED TO:
CHEMICAL ANALYSES
BUFFALO RIVER PILOT PROJECT
DATE:
CF#: 379GLBR
Dr. Steve Garbadak
Technical Project Manager
USEPA Great Lakes National Program Office
230 S. Dearborn
Chicago. IL 60604
INTRODUCTION
This report summarizes the results from analyses performed on pilot study samples
which were submitted by the U.S. Army Corps of Engineers Great Lakes Division.
Buffalo District.
SAHPIF CUSTODY
Samples were received 1n good condition from October 7. 1991 through November 25.
1991. Samples were logged 1n and stored as specified 1n the narrative accompanying
each method description. Samples were analyzed within the holding times specified
1n the QA plan. Any exceptions are noted 1n the narrative associated with each
analysis.
GRAIN SIZE
Seventeen samples were analyzed for grain size according to Battelle SOP# MSL-M-37
modified version of Plumb: 1981). The samples were separated Into four classes
(a
gravel, sand, silt and clay. Those classes (excluding
subdivided into 5 sand fractions. 6 silt fractions and
were stored at 4°+2°C prior to and following analysis.
duplicate) were archived and maintained at 4°+2° C for
future.
gravel) were further
4 clay fractions. Samples
Five samples (two 1n
possible analysis in the
Sponsor ID
070CT1.-221SCG
070CT12:511SBG
070CT12:161SAG
070CT1:561SDG
080CT5:222SD2G
D90CT12.-002SAG
090CT10:502SBG
090CT5:082SCG
230CT4:304SA2G
250CT9-.264SA3G
250CT2.-324SB1G
310CT9:274SB2G
310CT2:364SB3G
19NOV8:584SC1G
19NOV4:464SC2G
20NOV3:114SC3G
21NOV5:204SD1G
ARCHIVED SAMPLES
Sponsor ID
080CT5:232SD2G
080CT5:242SD2G
210CT6:024SA1G
19NOV4:464SC2G
19NOV4:464SC2G
22NOV3:124SD2G
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analvses
Grain Size
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Grain
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Size
Battelle ID
379GLBR*25
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
379GLBR'
'31
'32
'33
'47
'61
'69
'77
!120
:156
184
'219
'241
'299
'321
'346
'391
Analyses
Grain Size
Grain
Grain
Grain
Grain
Grain
Size
Size
Size
Size
Size
Battelle ID
379GLBRM7-T2
379GLBRM7-T3
379GLBR*94
379GLBR*321-T1
379GLBR*321-T2
379GLBRM20
-------
25NOV4:004SD3G
Sediment
Grain Size
379GLBRM46
Some values for % dry weight are greater than lOOfc due to absorption of moisture
during the cooling step of the method for determining % dry weight. If a
desiccator had been used, the samples would have exhibited % dry weight values -
99.5X. The analyst did not use a desiccator for the oven-drying step for the
determination of grain size. Therefore, when the analyst calculates the data, any
effect of moisture absorption 1s canceled out through the equations resulting 1n
valid data.
METALS
Forty-six sediment samples and1 thirty-three water samples were analyzed for metals.
The sediment samples were dried (Battelle SOP# MSL-M-3) and an aliquot was analyzed
by X-ray fluorescence for Cr. Cu and Pb. A separate dried aliquot was digested
with nitric, hydrofluoric and perchloric adds (Battelle SOP# MSL-M-7). then
analyzed for Hg by cold vapor atomic absorption (BatteUe SOP# MSL-M-31). An
aliquot of each water sample was digested with hot nitric add (Battelle SOP# MSL-M-
22) and analyzed by flame atomic absorption and graphite furnace atomic absorption
for Cr. Cu and Pb according to Battelle SOP# MSL-M-32 (based on EPA method 200.9).
A separate aliquot was digested with a solution of nitric and sulfuric add. then
analyzed for Hg by cold vapor atomic fluorescence following Battelle SOP# MSL-M-11.
According to the Buffalo River QA plan we were to analyze the Hg samples following
Battelle SOP# MSL-M-27 for Hg 1n water, however, due to the high content of
combustion by-products from organic contaminants 1t was necessary to treat these
samples as sediments. Thirteen sediment samples (3 in quadruplicate) and 12 water
samples (2 1n quadruplicate, 2 1n duplicate) were archived for possible analysis 1n
the future. Sediment samples were stored at -70°+10°C prior to drying. Once
dried, the samples were stored at room temperature prior to and following analysis.
Water samples were acidified at the time of collection and stored at room
temperature prior to and following analysis.
Sponsor ID
070CT1:261SCM
070CT12:191SAM
070CT2:001SDM
070CT12:541SBM
080CT4:572SDM
090CT12:002SAM
09DCT10:502SBM
090CT5:052SCM
220CT11:287SA1M
220CT11:358SA1M
230CT1:3D3SA2M
230CT4:314SA2M
240CT10:457SA2M
240CT10:508SA2M
240CT6-.203SA3M
250CT9:194SA3M
250CT9:287SA3M
250CT9:338SA3M
250CT2:153SB1M
250CT2:334SB1M
250CT3:517SB1M
250CT3:558SB1M
300CT4:463SB2M
310CT9:007SB2M
310CT9:088SB2M
310CT9:274SB2M
310CT2:384SB3M
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Battelle ID
379GLBR*26
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
379GLBR
27
28
29
49
60
68
76
103
106
115
119
135
138
146
150
155
168
177
186
192
195
207
208
211
215
245
-------
310CT10:453SB3M
1NOV10:208SB3M
1NOV10:157SB3M
18NOV4:4D3SC1M
19NOV8:484SC1M
19NOV9:218SC1M
19NOV9:327SC1M
19NOV3:553SC2M
19NOV4:414SC2M
20NOV8:157SC2M
20NOV1:553SC3M
20NOV3:184SC3M
20NOV3:327SC3M
20NOV3:268SC3M
21NOV2:433SD1M
21NOV4:578SD1M
21NOV5-.087SD1M
21NOV5:174SD1M
21NOV5:194SD1M
230CT4:459LA2M
230CT5:2510LA2M
230CT5:2010LA2M
250CT10:2010LA3M
250CT11:0010LA3M
250CT10:009LA3M
250CT3.-1210LB1M
250CT3:3D10LB1M
300CT4:216LA3M
310CT10:089LB2M
310CT10:2010LB2M
310CT10:3010LB2M
31DCT3:5010LB3M
310CT2:5710LB3M
310CT3:069LB3M
1NOV11:D06LB2M
1NOV2:506LB1B3M
6NOV12:003LM
18NOV5:309LC1M
18NOV6:1810LC1M
18NOV6:1810LC1M
19NOV5:559LC2M
19NOV5:2010LC2M
19NOV5-.3510LC2M
20NOV2:173LC3M
20NOV2:173LC3M
2DNOV2:439LC3M
20NOV3:0310LC3M
20NOV3:0710LC3M
21NOV3:3810LD1M
21NOV3:4510LD1M
21NOV4:359LD1M
"Samples were f1l
dissolved metals .
tSamples had a pH
ARCHIVED SAMPLES
Sponsor ID
070CT1:121SBM
080CT4:502SDM
080CT4:472SDM
080CT4:552SDM
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
on
Water
Water
Water
Water
011
Water
Water
Water
on
Water
Water
Water
Water
on
Water
Water
Water
011
Water
Water
on
Water
Water
Water
Water
on
Water
Water
Water
Water
on
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
tered at the time of collection
significantly greater
Sample Type
Sediment
Sediment
Sediment
'Sediment
than 2.
Analyses
Metals
Metals
Metals
Metals
379GLBR*246
379GLBR*265
379GLBR*267
379GLBR*285
379GLBR*300
379GLBR*305
379GLBR*308
379GLBR*316
379GLBR*320
379GLBR*336
379GLBR*345
379GLBR*353
379GLBR*356
379GLBR*359
379GLBR*361
379GLBR*383
379GLBR*386
379GLBR*389
379GLBR*390
379GLBR*127t
379GLBR*131t
379GLBRM33M
379GLBR*163t
379GLBRM70*
379GLBR*171t
379GLBR*188t
379GLBRM89*
379GLBR*203
379GLBR*223
379GLBR*228t
379GLBR*229*t
379GLBR*251*
379GLBR*254t
379GLBR*255
379GLBR*270
379GLBR*274
379GLBR*277
379GLBR'290t
379GLBR*292*
379GLBR*293
379GLBR*328t
379GLBR'333*
379GLBR*334
379GLBR*362*
379GLBR*363
379GLBR*368t
379GLBR*371
379GLBR*372*
379GLBR*399t
379GLBRMOO'
379GLBRM05t
therefore, results are for
Battelle ID
379GLBR*30
379GLBRM9-T2
379GLBRM9-T3
379GLBRM9-M1
-------
080CT4:522SDM
210CT12:503SA1M
210CT5:484SA1M
300CT4:493SB2M
300CT4.-503SB2M
300CT4:473SB2M
300CT4:483SB2M
19NOV4:414SC2M
19NOV4:414SC2M
19NOV4:414SC2M
19NOV4:414SC2M
22NOV1:453SD2M
22NOV3:184SD2M
22NOV3:164SD2M
22NOV3:348SD2M
25NOV2:203SD3M
25NOV4:004SD3M
25NOV4:004SD3M
210CT6:2510LA1M
210CT6:459LA1M
18NOV5:309LC1M
18NOV5:309LC1M
18NOV5:309LC1M
18NOV5:309LC1M
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:3510LC2M
19NOV5:3510LC2M
21NOV4.-359LD1M
21NOV4:359LD1M
21NOV4:359LD1M
21NOV4:359LD1M
22NOV2:3210LD2M
22NOV2:4010LD2M
22NOV2:559LD2M
25NOV4:0010LD3M
25NOV4:009LD3M
25NOV4:0010LD3M
"Samples were fil
dissolved metals .
tSamples had a pH
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Water
on
011
on
on
011
Water
Water
Water
Water
on
on
011
on
Water
Water
011
Water
Oil
Water
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
Metals
tered at the time of collection
significantly
greater than 2.
379GLBR'
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GIBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GIBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
379GLBR*
49-M2
81
86
207-T1
207-T2
207-M1
207-M2
320-T1
320-T2
320-M1
320-M2
413
421
422
425
441
442
448
96
102t
290-Tlt
290-T2t
290-Mlt
290-M2I
333-T2
333-M2
334-T1
334-T2
405-Tlt
405-T2I
405-Mlt
405-M2t
429t
430*
434t
455
4571
459
therefore results are for
Some samples were not acidified at the time of collection to a pH!2. Metals in
water samples stored for any period of time at a pH >2 tend to adsorb onto the
walls of the container which usually provide lower results. It became apparent in
March, after all samples had been analyzed, that some samples were not acidified
properly when mold was detected 1n those samples. We provided the acid normally
required to acidify freshwater samples to a pH<2. Therefore, either the acid was
not added to the sample or the alkalinity was so high in the sample that the amount
of add provide was not sufficient to bring the pH down to 2. Those samples have
been acidified since then and are available for re-analysis.
The water samples collected for metals analysis contained a high content of oil.
As Indicated by GLNPO. we digested the water including oil with hot nitric add to
obtain a total metals value. Values for samples flagged with an F represent total
dissolved metals 1n the entire sample (water + oil).
The high standard for lead in water has a concentration of 1 mg/L and a
mllHabsorbance reading of 47. Some water samples analyzed for lead had a
milHabsorbance reading slightly higher than 47 (48-55). The curve should still be
linear at these mllliabsorbance values, therefore would not affect the quality of
-------
the data. One sample had a mmlabsorbance reading of 66 which was diluted and
rerun by graphite furnace.
Deviations of the precision acceptance criteria for
that had concentrations near the detection limit of
higher chromium concentrations were well within the
established 1n the OA plan.
chromium were found on samples
25 ug/g. Samples that had
precision acceptance criteria
Water samples for mercury were analyzed by the water method Initially. As the
analyst became aware of matrix problems, she digested and analyzed all the samples
as sediments. The results on the first raw data sheet are for mercury by the water
method. Those results were not reported. When applicable, duplicate analyses were
averaged and the average was reported. Recoveries for one set of matrix spikes for
mercury 1n water were outside the criteria. Recoveries were high (128 and 155%)
due to very large dilution factors necessary to obtain results within the
calibration curve, however this should not compromise the data.
SOLIDS and TOC
Ninety-six sediment samples and twenty-two water samples were analyzed for solids
content and total organic carbon. An aliquot of each sample was oven-dried at
105°+5°C according to Battelle SOP# MSL-M-3. then taken to 550°+10°C to allow
volatilization according to Battelle SOP# MSL-M-2. A separate aliquot of each
sample was freeze-dried according to Battelle SOP# MSL-M-3 and sent to Global
Geochemistry Laboratory for total organic carbon analysis according to the LECO
method for TOC 1n weight percent. Water samples were analyzed for total solids
according to Battelle SOP// MSL-M-40 (based on Standard Methods. 2540B) and total
suspended solids according to Battelle SOP# MSL-M-39 (based on Standard Methods,
2540D). With such a high amount of heavy partlculates. 1t was difficult for the
analyst to obtain a representative sample for total suspended solids and total
solids. All solids samples were analyzed within the holding time of 7 days from
collection. However, if the reproduclbility was outside the acceptance criteria
of ±20% the samples were re-analyzed, usually after the holding time had been
exceeded. Separate samples collected at the sampling site were sent to Analytical
Resources. Inc. for total organic carbon. There was a problem with high
partlculate concentrations 1n the samples. After some discussion with Eric
Crecelius (program manager), they were instructed to allow the particulates to
settle, then withdraw a portion of the liquid phase for analysis.
Sponsor ID
070CT2:091SDS
070CT1:521SDS
D70CT1:111SBS
070CT1:201SCS
D70CT1:431SCS
070CT12:411SAS
070CT1:331SCS
070CT1:021SBS
070CT12:501SBS
070CT2:051SDS
070CT12.-321SAS
D70CT12:121SAS
080CT5:312SD2S
080CT5:412SD1S
080CT5:172SD3S
090CT11:282SA1S
090CT11:382SA2S
090CT11:502SA3S
090CT9:552SB1S
090CT10:152SB2S
090CT10:352SB3S
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
TS. TVS, TOC
TS. TVS, TOC
TS. TVS. TOC
TS. TVS, TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS, TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS, TOC
TS, TVS. TOC
TS, TVS. TOC
Battelle TD
379GLBR*34
379GLBR*35
379GLBR*36
379GLBR*37
379GLBR*38
379GLBR*39
379GLBRMO
379GLBRM1
379GLBRM2
379GLBRM3
379GLBRM4
379GLBRM5
379GLBRM8
379GLBR'50
379GLBR*52
379GLBR*54
379GLBR*55
379GLBR*56
379GLBR*62
379GLBR*63
379GLBR*64
-------
090CT4:362SC2S
090CT4:552SC1S
090CT4:152SC3S
220CT11:307SA1S
220CT11:368SA1S
220CT4:203SA2S
220CT5:553SA2S
230CT1:303SA20
230CT4:254SA2S
230CT4:264SA2S
230CT4:274SA2S
240CT10:457SA2S
240CT10:508SA2S
240CT2:203SA3S
240CT5:503SA3S
240CT6:203SA3S
250CT9:234SA3S
250CT9:244SA3S
250CT9:254SA3S
250CT9:307SA3S
250CT9:358SA3S
250CT12:153SB1S
300CT2:573SB2S
250CT2:153SB1S
250CT2:304SB1S
250CT2:314SB1S
250CT2:324SB1S
250CT3:517SB1S
250CT3:568SB1S
300CT4:053SB2S
300CT4:393SB2S
310CT9:D17SB2S
310CT9-.068SB2S
310CT9:204SB2S
310CT9:234SB2S
310CT9-.224SB2S
310CT2:364SB3S
310CT11:503SB3S
310CT10:453SB3S
310CT2:303SB3S
310CT2:374SB3S
310CT2:374SB3S
1NOV10:208SB3S
1NOV10:157SB3S
18NOV2:553SC1S
18NOV3:503SC1S
18NOV4:403SC1S
19NOV8:554SC1S
19NOV8:564SC1S
19NOV8:574SC1S
19NOV9.-228SC1S
19NOV9:337SC1S
19NOV11:303SC2S
19NOV2:203SC2S
19NOV3-.553SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4-.314SC2S
20NOV8:157SC2S
20NOV11:443SC3S
20NOV1.-003SC3S
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
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TS. TVS. TOC
TS. TVS. TOC
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TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS, TOC
TS. TVS. TOC
TS, TVS, TOC
TS. TVS. TOC
TS. TVS, TOC
TS. TVS, TOC
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS, TVS. TOC
TS, TVS. TOC
TS, TVS, TOC
TS. TVS, TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS, TVS. TOC
TS. TVS. TOC
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379GLBRVQ
379GLBR*71
379GLBR*72
379GLBR*98
379GLBRM05
379GLBR*109
379GIBRM10
379GLBR*114
379GLBR*116
379GLBR*117
379GLBR*118
379GLBR*134
379GLBR*137
379GLBRM40
379GLBRM42
379GLBR*144
379GLBR*147
379GLBR*148
379GLBR*149
379GLBR*157
379GLBRM69
379GLBR*173
379GLBR*172
379GLBRM75
379GLBRM78
379GLBRM79
379GLBR*180
379GLBRM91
379GLBR*194
379GLBR*200
379GLBR*205
379GLBR*209
379GLBR*212
379GLBR*216
379GLBR*217
379GLBR*218
379GLBR*235
379GLBR*236
379GLBR*237
379GLBR*238
379GLBR*239
379GLBR*Z40
379GLBR*264
379GLBR*266
379GLBR*279
379GLBR*281
379GLBR'283
379GLBR*296
379GLBR*297
379GLBR*296
379GLBR*306
379GLBR*309
379GLBR*310
379GLBR*312
379GIBR*314
379GLBR*317
379GLBR*318
379GLBR*319
379GLBR*338
379GLBR*339
379GLBR*341
-------
20NDV1:
20NOV3:
20NOV3:
20NOV3:
20NOV3:
20NOV3:
21NOV12
21NOV1:
21NOV2:
21NOV4:
21NOV5:
21NOV5:
21NOV5:
21NOY5:
553SC3S
124SC3S
124SC3S
124SC3S
317SC3S
258SC3S
:003SD1S
353SD1S
433SD1S
558SD1S
087SD1S
214SD1S
214SD1S
214SD1S
230CT4:459LA2S
230CT5:2010LA2S
250CT10:2210LA3S
250CT10:2110LA3S
250CT3:1110LB1S
300CT4:166LA3S
310CT10:059LB2S
310CT10:1910LB2S
310CT2:5410LB3S
310CT2:5610LB3S
310CT3:049LB3S
310CT3:059LB3S
6NOV12:003LS
18NOV5:409LC1S
18NOV6:1010LC1S
19NOV5:539LC2S
19NOV5:2410LC2S
20NOV2:163LC3S
20NOV2:4D9LC3S
20NOV3.-0010LC3S
21NOV3:3510LD1S
21NOV4:039LD1S
30CT4:459LA20
230CT5:2010LA2C
25DCT10:2110LA3C
250CT10:009LA3C
250CT3:1110LB1C
300CT4:206LA3C
310CT10:109LB2C
310CT1D:2410LB2C
310CT2:5810LB3C
310CT3:099LB3C
1NOV11:006LB2C
1NOV2:506LB1B3C
6NOV12:003LC
18NOV6:0610LC1C
18NOV5:459LC1C
19NOV5:579LC2C
19NOV5:4310LC2C
20NDV2.-183LC3C
20NOV2:449LC3C
20NOV3:0210LC3C
21NOV3:3710LD1C
21NOV4:459LD1C
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
011
Water
Water
Water
Water
Water
011
Water
Water
Water
011
011
Water
011
Water
011
Water
Water
on
Water
Water
011
on
Water
Water
011
Water
Water
011
Water
Water
011
Water
Water
Water
Water
011
011
Water
Water
011
Water
Water
on
TS, TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
TS. TVS. TOC
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TS. TSS
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TS. TSS
TS. TSS
TS. TSS
TS, TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS. TSS
TS, TSS
TS, TSS
TS, TSS
TS, TSS
TS. TSS
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
TOC
379GLBR*343
379GLBR*347
379GLBR*348
379GLBR*349
379GLBR*355
379GLBR*358
379GLBR*375
379GLBR*377
379GLBR*379
379GLBR*382
379GLBR*387
379GIBR*392
379GLBR*393
379GLBR*394
379GLBR*126
379GLBRM30
379GLBR*158
379GLBR*159
379GLBR*197
379GLBR*202
379GLBR*224
379GLBR*230
379GLBR*258
379GLBR*259
379GLBR*260
379GLBR*261
379GLBR*276
379GLBR*289
379GLBR*291
379GLBR*329
379GLBR*332
379GLBR*364
379GLBR*367
379GLBR*373
379GLBRM01
379GLBRM03
379GLBR*125
379GLBR*129
379GLBRM62
379GLBRM65
379GLBRM90
379GLBR*201
379GLBR*225
379GLBR*231
379GLBR*262
379GLBR*263
379GLBR*271
379GLBR*273
379GIBR*278
379GLBR*294
379GLBR'295
379GLBR*330
379GLBR*335
379GLBR*365
379GLBR*369
379GLBR*374
379GLBRM02
379GLBRM06
-------
BUFFALO PILOT PROJECT (CF# 379)
GRAIN SIZE - TOTAL SOLIDS ANALYSIS
MSLCode
379GLBR-32
379GLBR-61
379GLBR-120
379GLBR-156
379GLBR-31
379GLBR-69
379GLBR-184
379GLBR-219
379GLBR-241
379GLBR-25
379GLBR-77
379GLBR-299
379GLBR-321
379GLBR-321
379GLBR-321
379GLBR-346
379GLBR-33
379GLBR-47
379GLBR-47
379GLBR-47
379GLBR-391
379GLBR-346
379GLBR-391
Sponsor ID
. c
07OCT12:161SAG
09OCT12:002SAG
23OCT4:304SA2G
25OCT9:264SA3G
C
07OCT12:511SBG
09OCT10:502SBG
25OCT2.-324SB1G
31OCT9:274SB2G
31OCT2:364SB3G
c
07OCT1:221SCG
09OCT5:082SCG
19NOV8:584SC1G
Rep1 19NOV4:464SC2G
Rep 2 19NOV4:464SC2G
Rep 3 19NOV4:464SC2G
20NOV3:114SC3G
c
07OCT1:561SDG
Rep 1 080CT5:222SD2G
Rep 2 08OCT5:222SD2G
Rep 3 08OCT5:222SD2G
21NOV5:204SD1G
20NOV3:114SC3G
21NOV5:204SD1G
% Total
Solids
-
BIN A I
60.05%
64.44%
99.87%
99.55%
BIN B I
54.78%
59.75%
98.94%
100.09%
100.01%
BIN C |
65.29%
60.00%
100.05%
100.11%
100.14%
100.14%
96.79%
BIN D |
59.83%
75.50%
58.80%
58.80%
99.97%
96.79%
99.93%
Predicted
Dry
Mass (q)
14.2368
13.5706
10.4067
9.2782
14.4168
12.2001
9.3495
9.5281
9.8506
14.5604
11.9039
10.3054
9.8212
9.8535
9.9439
9.4950
13.2771
14.6170
11.3138
11.4663
9.2072
9.4950
10.2629
Actual
Dry
Mass(q)
15.2327
13.7666
10.0779
10.2376
15.7037
13.2007
10.1831
10.1853
10.5914
15.0865
13.0577
10.4093
10.4951
10.3475
10.5172
10.1702
14.1625
12.6762
12.5171
12.4534
10.0154
10.1720
10.8617
Estimated
Recovery
107.00%
1 01 .44%
96.84%
110.34%
108.93%
108.20%
108.92%
106.90%
107.52%
103.61%
109.69%
101.01%
106.86%
105.01%
105.77%
107.11%
106.67%
86.72%
110.64%
108.61%
108.78%
107.11%
105.83%
These dry samples were not disaggregated before analysis was done.
They should be used only as a comparison for the rest of the
dry samples which were disaggregated before analysis.
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
GRAIN SIZE - TOTAL SOUDS ANALYSIS
PERCENT OF TOTAL MASS
MSI Code
BIN A I
379GLBR-32
379GLBR-61
379GLBR-120
379GLBR-156
BINB |
379GLBR-31
379GLBR-69
379GLBR-184
379GLBR-219
379GLBR-241
BINC |
379GLBR-25
379GLBR-77
379GLBR-299
379GLBR-321 Rep
379GLBR-321 Rep
379GLBR-321 Rep
379GLBR-346
BIND I
379GLBR-33
379GLBR-47 Rep
379GLBR-47 Rep
379GLBR-47 Rep
379GLBR-391
379GLBR-346 *
379GLBR-391 *
1.00-
Sponsor ID >2.00 mm 2.00 mm 1
07OCT12:161SAG
09OCT12:002SAG
23OCT4:304SA2G
25OCT9:264SA3G
07OCT12:511SBG
09OCT10:502SBG
25OCT2:324SB1G
31OCT9:274SB2G
31OCT2:364SB3G
07OCT1221SCG
09OCT5:082SCG
19NOV8:584SC1G
1 19NOV4:464SC2G
2 19NOV4:464SC2G
3 19NOV4:464SC2G
20NOV3:114SC3G
070CT1:561SDG
1 08OCT5:222SD2G
2 08OCT5:222SD2G
3 08OCT5:222SD2G
21NOV5:204SD1G
20NOV3:114SC3G
21NOV5:204SD1G
0.06
0.40
0.00
0.00
0.08
0.13
0.04
0.00
0.04
0.10
0.08
0.00
0.00
0.11
0.00
0.27
0.10
0.02
0.09
0.82
0.00
30.59
33.61
0.11
0.05
0.21
0.38
0.06
0.14
0.16
0.24
0.19
0.13
0.14
0.31
0.39
0.07
0.11
0.66
0.05
0.09
0.14
0.16
0.14
15.06
17.82
0.500- 0.25- 0.125-
.00 mm 0.500 mm 0.250 mm 0.
0.15
0.20
0.38
0.91
0.22
0.27
0.36
0.33
0.59
0.23
0.20
0.42
0.34
0.48
0.45
0.98
0.14
0.32
0.26
0.25
0.66
9.86
11.90
0.53
1.12
1.91
1.28
0.66
1.48
1.86
2.06
3.18
1.45
1.09
2.17
3.24
3.56
3.90
2.52
0.73
1.13
1.17
1.10
4.40
4.84
5.37
2.67
3.83
4.75
3.85
1.78
4.90
9.10
7.65
6.03
15.60
4.86
8.53
13.37
10.75
10.24
8.44
4.33
3.61
3.88
3.54
8.32
5.79
3.97
0.0625- 48.0- 31.2-
125 mm 62.5 urn 48.0 um
10.29
12.19
14.32
13.25
7.46
13.75
16.40
17.86
16.82
15.58
13.74
18.63
14.17
17.68
17.52
17.27
13.79
12.76
12.50
12.58
16.38
7.78
6.34
3.73
3.60
2.58
6.90
4.79
3.30
2.51
9.90 '
1.40
1.22
4.56
7.99
5.49
8.39
6.28
6.88
3.39
4.23
2.05
2.18
2.16
1.24
2.03
6.38
5.99
11.23
8.38
3.23
7.55
11.51
6.99
8.84
7.87
5.76
7.38
8.65
7.19
9.28
7.98
8.08
7.57
7.22
8.87
8.43
3.14
1.84
NOTE: All results are in percent.
* These dry samples were not disaggregated before analysis was done.
They should be used only as a comparison for the rest of the
dry samples which were disaggregated before analysis.
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
GRAIN SIZE - TOTAL SOLIDS ANALYSIS
PERCENT OF TOTAL MASS
MSLCode
BIN A I
379GLBR-32
379GLBR-61
379GLBR-120
379GLBR-156
! BIN B I
379GLBR-31
379GLBR-69
379GLBR-184
379GLBR-219
379GLBR-241
BINC I
379GLBR-25
379GLBR-77
379GLBR-299
379GLBR-321 Rep 1
379GLBR-321 Rep 2
379GLBR-321 Rep 3
379GLBR-346
BIND I
379GLBR-33
379GLBR-47 Rep 1
379GLBR-47 Rep 2
379GLBR-47 Rep 3
379GLBR-391
379GLBR-346 *
379GLBR-391 *
Sponsor ID
07OCT12:161SAG
09OCT12:002SAG
23OCT4:304SA2G
25OCT9:264SA3G
07OCT12:511SBG
09OCT10:502SBG
25OCT2:324SB1G
31OCT9:274SB2G
31OCT2:364SB3G
07OCT1:221SCG
09OCT5:082SCG
19NOV8:584SC1G
19NOV4:464SC2G
19NOV4:464SC2G
19NOV4:464SC2G
20NOV3:114SC3G
070CT1:561SDG
08OCT5:222SD2G
08OCT5:222SD2G
08OCT5:222SD2G
21NOV5:204SD1G
20NOV3M14SC3G
21NOV5:204SD1G
23.0-
31.2 urn
10.50
8.08
11.35
10.79
10.49
8.09
10.29
10.17
9.44
6.95
10.14
7.92
8.16
7.38
8.10
8.14
8.08
7.76
9.65
8.42
8.55
1.98
2.25
15.6-
23.0 urn
10.61
10.87
11.35
11.65
10.55
9.48
8.60
9.86
8.76
8.46
9.59
7.99
7.47
7.50
7.53
7.35
10.20
10.67
9.81
11.15
10.78
3.29
2.32
7.8-
15.6 urn
20.06
17.84
19.85
21.89
21.17
17.21
14.02
15.16
23.79
12.20
16.76
21.17
15.51
14.61
13.92
16.91
18.08
16.82
17.70
17.18
20.45
6.78
5.08
3.9-
7.8 um
10.48
9.24
8.57
2.96
12.00
8.48
8.68
8.25
8.57
9.68
8.73
2.96
7.55
6.84
6.47
7.91
9.46
9.09
8.66
9.06
8.07
2.90
1.58
1.9-
3.9 um
7.59
6.57
6.03
4.75
8.35
6.39
5.66
5.07
5.36
5.30
5.67
7.72
9.68
5.03
5.25
5.03
6.44
6.41
6.20
6.33
4.75
1.34
0.88
0.976- 0.488- Sa/f Blank
1.9 um 0.976 um <0.488 um (a)
5.17
4.68
3.81
6.66
5.09
4.85
4.24
3.50
0.04
3.37
4.07
0.77
3.28
8.12
8.48
3.85
4.80
4.29
4.44
4.53
3.99
0.99
0.48
3.12
3.31
2.66
0.43
3.72
3.2" 1
0.86
1.96
2.04
2.81
3.37
3.34
0.95
0.89
0.65
4.88
3.50
3.41
3.32
3.31
2.12
0.14
0.37
8.38
12.03
0.99
5.92
10.34
10.76
5.70
' 1.02
4.91
9.07
11.24
2.69
1.75
1.39
1.83
0.90
8.84
11.83
12.91
10.54
0.80
4.28
4.16
0.0158
0.0072
0.0009
0.0005
0.0111
0.0109
0.0004
0.0003
0.0005
0.0119
0.0105
0.0004
0.0006
0.0011
0.0007
0.0003
0.0156
0.0098
0.0087
0.0157
0.0006
0.0222
0.0191
NOTE: All results are in percent.
* These dry samples were not disaggregated before analysis was done.
They should be used only as a comparison for the rest of the
dry samples which were disaggregated before analysis.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 8
379GLBR- 27
379GLBR- 60
379GLBR- 103
379GLBR- 106
379GLBR- 115
379GLBR- 119
379GLBR- 135
379GLBR- 138
379GLBR- 146
379GLBR- 150
379GLBR- 154
379GLBR- 155
379GLBR- 168
379GLBR- 462
379GLBR- 29
379GLBR- 68
379GLBR- 177
379GLBR- 186
379GLBR- 192
379GLBR- 195
379GLBR- 207 Rep 1
379GLBR- 207 Rep 2
379GLBR- 207 Rep 3
379GLBR- 208
379GLBR- 211
379GLBR- 215
379GLBR- 245
379GLBR- 246
379GLBR- 265
379GLBR- 267
Sponsor ID
| ' BIN A
07OCT1 2:301 SAL
07OCT12:191SAM
09OCT12:002SAM
22OCT1 1 :287SA1 M
22OCT11:358SA1M
23OCT1 :303SA2M
23OCT4:314SA2M
24OCT1 0:457SA2M
24OCT10:508SA2M
240CT6:203SA3M
25OCT9:194SA3M
25OCT9:104SA3M
25OCT9:287SA3M
25OCT9:338SA3M
4DEC12:055SA2M
I BIN B
07OCT1 2:541 SBM
090CT10:502SBM
25OCT2:153SB1M
25OCT2:334SB1M
25OCT3:517SB1M
25OCT3:558SB1M
30OCT4:463SB2M
30OCT4:463SB2M
30OCT4:463SB2M
31OCT9:007SB2M
31OCT9:088SB2M
31OCT9:274SB2M
31OCT2:384SB3M
31OCT10:453SB3M
1NOV10:208SB3M
1NOV10:157SB3M
Cr (ug/g)
XFF
I
77
73
60
110
155
47
70
137
84
68
61
66
148
88
100
I
63
51
47
56
129
121
46
70
57
106
77
44
58
55
117
130
Cu (ug/g)
WF
39.8
46.2
45.8
55.3
55.4
41.1
38.2
51.3
42.3
40.6
41.3
42.7
47.1
43.1
41.6
41.0
43.0
37.6
45.7
48.2
46.2
44.9
41.1
43.0
46.8
47.1
45.6
44.1
43.2
49.5
47.8
Pb (ug/g)
VFF
46.0
72.2
52.4
65.6
56.6
53.7
52.1
58.9
48.8
52.4
52.7
54.9
56.7
48.0
50.5
49.3
58.2
64.3
65.7
65.1
58.4
65.7
56.4
62.9
67.0
64.5
67.0
61.1
60.6
61.3
62.3
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 26
379GLBR- 76
379GLBR- 285
379GLBR- 300
379GLBR- 305
379GLBR- 308
379GLBR- 316
379GLBR- 320 Rep 1
379GLBR- 320 Rep 2
379GLBR- 320 Rep 3
379GLBR- 336
379GLBR- 345
379GLBR- 353
379GLBR- 356
379GLBR- 359
379GLBR- 28
379GLBR- 49 Rep 1
379GLBR- 49 Rep 2
379GLBR- 49 Rep 3
379GLBR- 381
379GLBR- 383
379GLBR- 386
379GLBR- 390
Sponsor ID
I . BIN C
07OCT1261SCM
09OCT5:052SCM
18NOV4:403SC1M
19NOV8:484SC1M
19NOV9:218SC1M
19NOV9:327SC1M
19NOV3:553SC2M
19NOV4:414SC2M
19NOV4:414SC2M
19NOV4:414SC2M
20NOV8:157SC2M
20NOV1 :553SC3M
20NOV3:184SC3M
20NOV3:327SC3M
20NOV3:268SC3M
I BIND
07OCT2:001SDM
08OCT4572SDM
08OCT4:572SDM
08OCT4:572SDM
21NOV2:43ESD1M
212NOV4:578SD1M
21NOV5.-087SD1M
21NOV5:194SD1M
Cr (ug/g) Cu
I
80
71
73
67
129
136
59
75
63
37
129
69
62
140
140
I
74
49
56
76
55
118
112
62
(ug/g)
56.8
47.8
45.3
58.0
62.1
54.8
48.2
47.6
51.4
47.4
56.1
47.2
45.4
62.4
52.5
37.7
44.5
42.8
47.1
44.8
53.7
51.3
47.6
Pb (ug/g)
88.8
62.3
68.4
70.6
59.7
83.8
71.9
68.6
67.4
65.5
70.7
56.3
58.3
70.4
61.7
49.7
65.0
60.3
61.7
73.5
71.8
63.6
64.7
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN SEDIMENT SAMPLES
MSLCode
STANDARD
SRM 1646
SRM 1646
SRM 1646
SRM1646
SRM 2704
SRM 2704
SRM 2704
Sponsor ID
REFERENCE MATERIAL
Rep1 :
Rep 2
Rep 3
Rep 4
certified
value
Rep 1
Rep 2
Rep 3
certified
value
Cr (ug/g)
XRF
61
78
78
72
76
±3
140
134
139
135
±5
Cu (ug/g)
XHF
22.1
19.7
23.2
20.9
18
±3
91.6
97.5
92.9
98.6
±5.0
Pb (ug/g)
XRF
26.9
28.3
29.1
29.3
28.2
±1.8
156.5
156.2
155.1
161.0
±17.0
REPLICATE ANALYSIS
379GLBR- 207 Rep 1
379GLBR- 207 Rep 2
379GLBR- 207 Rep 3
379GLBR- 320 Rep 1
379GLBR- 320 Rep 2
379GLBR- 320 Rep 3
379GLBR- 49 Rep 1
379GLBR- 49 Rep 2
379GLBR- 49 Rep 3
30OCT4:463SB2M
300CT4:463SB2M
300CT4:463SB2M
RSD %
19NOV4:424SC2M
19NOV4:424SC2M
19NOV4-.424SC2M
RSD %
08OCT4:572SDM
08OCT4:572SDM
08OCT4:572SDM
RSD %
46
70
57
21%
75
63
37
33%
49
56
76
23%
44.9
41.1
43
4%
47.6
51.4
47.4
5%
44.5
42.8
47.1
5%
65.7
56.4
62.9
8%
68.6
67.4
65.5
2%
65
60.3
61.7
4%
RSD % = Relative Standard Deviation.
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN SEDIMENT SAMPLES
MSLCode
379GLBR- 8
379GLBR- 27
379GLBR- 60
379GLBR- 103
379GLBR- 106
379GLBR- 115
379GLBR- 119
379GLBR- 135
379GLBR- 138
379GLBR- 146
379GLBR- 150
379GLBR- 154
379GLBR- 155
379GLBR- 168
379GLBR- 462
379GLBR- 29
379GLBR- 68
379GLBR- 177
379GLBR- 186
379GLBR- 192
379GLBR- 195
379GLBR- 207 Rep 1
379GLBR- 207 Rep 2
379GLBR- 207 Rep 3
379GLBR- 208
379GLBR- 211
379GLBR- 215
379GLBR- 245
379GLBR- 246
379GLBR- 265
379GLBR- 267
Sponsor ID
I * BIN A |
: 07OCT1 2:301 SAL
07OCT12:191SAM
090CT12:002SAM
22OCT11:287SA1M
22OCT11:358SA1M
23OCT1 :303SA2M
23OCT4:314SA2M
24OCT10:457SA2M
24OCT10:508SA2M
24OCT6:203SA3M
25OCT9:194SA3M
25OCT9:L104SA3M
25OCT9:287SA3M
250CT9:338SA3M
4DEC12:055SA2M
| BIN B |
070CT1 2:541 SBM
09OCT10:502SBM
25OCT2:153SB1M
25OCT2:334SB1M
25OCT3:517SB1M
25OCT3:558SB1M
30OCT4:463SB2M
30OCT4:463SB2M
30OCT4:463SB2M
31OCT9:007SB2M
31OCT9:088SB2M
31OCT9:274SB2M
31OCT2:384SB3M
31OCT10:453SB3M
1NOV10:208SB3M
1NOV10:157SB3M
Hg (ug/g)
CVAA
0.112
0.183
0.192
0.183
0.089
0.171
0.002
0.146
0.023
0.175
0.045
0.027
0.120
0.036
0.017
0.170
0.208
0.203
0.111
0.132
0.121
0.190
0.205
0.203
0.102
0.023
<0.0003
0.032
0.173
0.084
0.175
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN SEDIMENT SAMPLES
MSLCode
379GLBR- 23
379GLBR- 76
379GLBR- 285
379GLBR- 300
379GLBR- 305
379GLBR- 308
379GLBR- 316
379GLBR- 320 Rep 1
379GLBR- 320 Rep 2
379GLBR- 320 Rep 3
379GLBR- 336
379GLBR- 345
379GLBR- 353
379GLBR- 356
379GLBR- 359
379GLBR- 28
379GLBR- 49 Rep 1
379GLBR- 49 Rep 2
379GLBR- 49 Rep 3
379GLBR- 381
379GLBR- 383
379GLBR- 386
379GLBR- 390
Blank Rep 1
Blank Rep 2
Blank Rep 3
Blank Rep 4
Blank Rep 5
Sponsor ID
-
| BINC
07OCT1261SCM
09OCT5:052SCM
18NOV4.-403SC1M
19NOV8:484SC1M
19NOV9:218SC1M
19NOV9:327SC1M
19NOV3:553SC2M
19NOV4:414SC2M
19NOV4:414SC2M
19NOV4:414SC2M
20NOV8:157SC2M
20NOV1 :553SC3M
20NOV3:184SC3M
20NOV3:327SC3M
20NOV3:268SC3M
I BIN D |
07OCT2.-001SDM
080CT4:572SDM
08OCT4.-572SDM
080CT4:572SDM
21NOV2:433SD1M
21NOV4:578SD1M
21NOV5:087SD1M
21NOV5:194SD1M
Hg (ug/g)
CVAA
0.335
0.198
0.202
0.065
0.300
0.323
0.213
0.046
0.054
0.052
0.228
0.175
0.151
0.487
0.060
0.110
0.214
0.207
0.233
0.187
0.034
0.209
0.014
<0.0003
<0.0003
<0.0003
<0.0003
<0.0003
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN SEDIMENT SAMPLES
MSLCode Sponsor ID
STANDARD REFERENCE MATERIAL
SRM 1646 Rep 1
SRM 1646 Rep 2
SRM 1646 Rep 3
SRM 1646 Rep 4
certified
value
SRM 2704 Rep 1
SRM 2704 Rep 2
SRM 2704 Rep 3
certified
value
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-8 070CT1 2:301 SAL
379GLBR-8 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-8 DUPLICATE
379GLBR-8 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-49 08OCT4:572SDM
379GLBR-49 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-49 DUPLICATE
379GLBR-49 + Spike
Amount Recovered
Percent Recovery
Hg (ug/g)
CVAA
0.072
0.076
0.070
0.066
0.063
±0.012
1.434
1.439
1.450
1.44
±0.07
0.500
0.112
0.647
0.535
107%
0.500
0.112
0.667
0.555
111%
0.500
0.214
0.649
0.435
87%
0.500
0.207
0.639
0.432
86%
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN SEDIMENT SAMPLES
MSLCode
Sponsor ID
Hg (ug/g)
CVAA
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-207
379GLBR-207+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-207 DUPLICATE
379GLBR-207+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-320
379GLBR-320+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-320 DUPLICATE
379GLBR-320+ Spike
Amount Recovered
Percent Recovery
30OCT4:463SB2M
19NOV4:424SC2M
0.500
0.190
0.703
0.513
103%
0.500
0.205
0.659
0.454
91%
0.500
0.046
0.501
0.455
91%
0.500
0.054
0.516
0.462
92%
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN SEDIMENT SAMPLES
MSLCode
Sponsor ID
HQ (ug/g)
CVAA
REPLICATE ANALYSIS
379GLBR- 207 Rep 1
379GLBR- 207 Rep 2
379GLBR- 207 Rep 3
379GLBR- 320 Rep 1
379GLBR- 320 Rep 2
379GLBR- 320 Rep 3
379GLBR- 49 Rep 1
379GLBR- 49 Rep 2
379GLBR- 49 Rep 3
30OCT4:463SB2M
300CT4:463SB2M
30OCT4:463SB2M
RSD%
19NOV4:424SC2M
19NOV4:424SC2M
19NOV4:424SC2M
RSD%
08OCT4572SDM
08OCT4572SDM
08OCT4:572SDM
RSD%
0.190
0.205
0.203
4%
0.046
0.054
0.052
8%
0.214
0.207
0.233
6%
RSD % - Relative Standard Deviation.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSL Code Sponsor ID
MDL • Flame AA
MDL • Graphite Furnace AA
Cr
ug/L
40
0.22
Cu
ug/L
50
0.72
Pb
ug/L
100
1.03
BIN A
379GLBR- 127
379GLBR- 131
379GLBR- 133 REP 1
379GLBR- 133 REP 2
379GLBR- 133 REP 3
379GLBR- 163
379GLBR- 170
379GLBR- 171
379GLBR- 203
379GLBR- 188
379GLBR- 189
379GLBR- 223
379GLBR- 228
379GLBR- 229 REP 1
379GLBR- 229 REP 2
379GLBR- 229 REPS
379GLBR- 251
379GLBR- 254
379GLBR- 255
379GLBR- 270
379GLBR- 274
379GLBR- 290
379GLBR- 292
379GLBR- 293
379GLBR- 328
379GLBR- 333 REP 1
379GLBR- 333 REP 2
379GLBR- 333 REP 3
379GLBR- 334
379GLBR- 362
379GLBR- 363
230CT4:459LA2M
23OCT5:2510LA2M
23OCT5:2010LA2M
23OCT5:2010LA2M
23OCT5:2010LA2M
25OCT1 0:201 OLA3M
25OCT11:0010LA3M
25OCT10:009LA3M
30OCT4:216LA3M
I BIN B |
25OCT3:1210LB1M
25OCT3:3010LB1M
31OCT10:089LB2M
31OCT10:2010LB2M
31 OCT1 0:301 OLB2M
31 OCT1 0:301 OLB2M
31 OCT1 0:301 OLB2M
31OCT3:5010LB3M
31OCT2:5710LB3M
31OCT3:069LB3M
1NOV11:006LB2M
1NOV2:506LB1B3M
I BIN C |
18NOV5:309LC1M
18NOV6:1810LC1M
18NOV6:1810LC1M
19NOV5:559LC2M
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:3510LC2M
20NOV2:173LC3M
20NOV2.-173LC3M
13130
1080
4.15'
4.40 *
4.15*
600
2.89 *
14200
1.13 *
1870
2.52 *
22.4 *
200
1.76*
1.76*
1.76 *
1.76 *
270
120
2.39 *
1.51 *
830
2.77 *
230
410
1.64*
1.64 *
2.14 *
160
1.51 *
1.51 *
25590
1350
830
830
820
570
410
7100
4.17*
840
340
2800
560
450
450
450
330
520
1830
5.83*
14.2 *
3660
720
1410
2220
120
110
120
260
5.00*
7.91 *
12600
1040
2.97 *
2.97*
3.56 *
230
1.19 *
7100
1.19*
900
3.56*
32.6*
154 *
1.78*
2.37*
2.37*
25.5 *
200
140
1.19 *
1.19 *
810
1.78 *
330
410
13.1 *
14.2 *
14.8 *
180
2.37 *
4.15 *
F
F
F
F
F
F
F
F
F
F
F
F
F
F
NOTE: Sample values are not blank-corrected.
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSLCode Sponsor ID
MDL - Flame AA
MDL - Graphite Furnace AA
Cr
ug/L
40
0.22
Cu
ug/L
50
0.72
Pb
ug/L
100
1.03
BINC
379GLBR- 368
379GLBR- 371
379GLBR- 372
379GLBR- 399
379GLBR- 400
379GLBR- 405 REP 1
379GLBR- 405 REP 2
379GLBR- 405 REPS
379GLBR- 429
379GLBR- 430
379GLBR- 434
379GLBR- 457
20NOV2:43&LC3M
20NOV3:0310LC3M
20NOV3:0710LC3M
| BIND
21NOV3:3810LD1M
21NOV3:4510LD1M
21NOV4:359LD1M
21NOV4:359LD1M
21NOV4:359LD1M
22NOV2:3210LD2M
22NOV2:4010LD2M
22NOV2:559LD2M
25NOV4:009LD3M
| DILUTION WATER
1140
170
1.01 *
I
340
1.64 *
800
620
750
530
2.52*
840
790
1010
190
70
860
755'
1950
1950
1950
950
630
1310
3000
19.6
160
17.8
250
8.90
580
560
560
440
9.49
540
1620
379GLBR- 277
6NOV12:003LM
2.26 *
17.9
2.37'
Blank
Blank
Blank
Blank
Blank
Blank
Blank
Blank
Rep 1
Rep 2
Rep 3
Rep 4
Rep1
Rep 2
Rep 3
Rep 4
(Flame AA)
(Graphite Furnace AA)
40 U
40 U
40 U
40 U
1.13 *
6.67 '
1.01 *
1.13 *
50 U
50 U
50 U
50 U
4.17*
4.17 *
3.33 *
4.58 *
100 U
100 U
100 U
100 U
1.03 U1
1.03 U'
1.03 U'
1.03 U'
NOTE: Sample values are not blank-corrected.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSLCode Sponsor ID
MDL • Flame AA
MDL • Graphite Furnace AA
Cr
ug/L
40
0.22
Cu
ug/L
so
0.72
Pb
ug/L
100
1.03
STANDARD REFERENCE MATERIAL
SRM 1643C
SRM 1643C
SRM 1643C
SRM 1643C
Rep 1
Rep 2
Rep 3
Rep 4
NOTE: SRM values are not blank-corrected.
MATRIX SPIKE RESULTS - FLAME AA
Amount Spiked
379GLBR- 203
379GLBR- 203 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 203
379GLBR- 203 + Spike DUPLICATE
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 274
379GLBR- 274 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 274
379GLBR- 274 + Spike DUPLICATE
Amount Recovered
Percent Recovered
NOTE: Spike data run by Flame AA is not blank-corrected.
21.5 *
21. 5 •
19.1 *
20.4 *
19.0
±0.6
1000
40 U
940
940
94%
1000
40 U
890
890
89%
1000
40 U
890
890
89%
1000
40 U
1020
1020
102%
29.2"
26.7 *
28.7 •
27.1 •
22.3
±2.8
1000
50 U
1030
1030
103%
1000
50
1050
1050
105%
1000
50 U
990
990
99%
1000
50 U
1140
1140
114%
35.6 *
36.8*
36.8 *
33.8 *
35.3
±0.9
1000
100 U
1080
1080
108%
1000
100 U
1060
1060
106%
1000
100 U
1010
1010
101%
1000
100 U
1110
1110
111%
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSLCode Sponsor ID
MDL • Flame AA
MDL • Graphite Furnace AA
Cr
ug/L
40
0.22
Cu
ug/L
50
0.72
Pb
ug/L
100
1.03
Amount Spiked
379GLBR- 362
379GLBR- 362 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 362
379GLBR- 362 + Spike DUPLICATE
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 400
379GLBR- 400 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 400
379GLBR- 400 + Spike DUPLICATE
Amount Recovered
Percent Recovered
NOTE: Spike data run by Flame AA is not blank-corrected
MATRIX SPIKE RESULTS - GRAPHITE FURNACE AA
Amount Spiked
379GLBR- 203
379GLBR- 203 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 203
379GLBR- 203 + Spike DUPLICATE
Amount Recovered
Percent Recovered
NOTE: Spike data run by Graphite Furnace AA is blank-corrected.
Page 4
1000
40 U
1030
1030
103%
1000
40 U
1040
1040
104%
1000
40 U
1040
1040
104%
1000
40 U
1040
1040
104%
corrected
AA
1000
0.22 U
1091
1091
109%
1000
0.22 U
1062
1062
106%
1000
50 U
1020
1020
102%
1000
50 U
1040
1040
104%
1000
330
1360
1030
103%
1000
330
1370
1040
104%
1000
0.72 U
1110
1110
111%
1000
0.72 U
977
977
98%
1000
100 U
1000
1000
100%
1000
100 U
980
980
98%
1000
100 U
1020
1020
102%
1000
100 U
980
980
98%
1000
1.19
919
917
92%
1000
1.19
912
911
91%
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSLCode Sponsor ID
MDL • Flame AA
MDL • Graphite Furnace AA
Amount Spiked
379GLBR- 274 ;
379GLBR- 274 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 274
379GLBR- 274 + Spike DUPLICATE
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 362
379GLBR- 362 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 362
379GLBR- 362 + Spike DUPLICATE
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 400
379GLBR- 400 + Spike
Amount Recovered
Percent Recovered
Amount Spiked
379GLBR- 400
379GLBR- 400 + Spike DUPLICATE
Amount Recovered
Percent Recovered
Cr
ug/L
40
0.22
1000
0.38
1120
1120
112%
1000
0.38
1152
1152
115%
1000
0.38
1052
1052
105%
1000
0.38
1023
1023
102%
1000
0.50
1101
1100
1 1 0%
1000
0.50
1110
1110
111%
Cu
ug/L
50
0.72
1000
10.0
933
923
92%
1000
10.0
1066
1056
106%
1000
0.83
1155
1154
115%
1000
0.83
1066
1065
107%
1000
577
1421
844
84%
1000
577
1643
1066
107%
Pb
ua/L
100
1.03
1000
1.19
1057
1055
106%
1000
1.19
1057
1055
106%
1000
2.37
977
974
97%
1000
2.37
957
955
95%
1000
8.90
983
974
97%
1000
8.90
964
955
95%
NOTE: Spike data run by Graphite Furnace AA is blank-corrected.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN WATER SAMPLES
MSLCode Sponsor ID
MDL • Flame AA
MDL - Graphite Furnace AA
Cr
ug/L
40
0.22
Cu
ug/L
50
0.72
Pb
ug/L
100
1.03
REPLICATE ANALYSIS
379GLBR- 130 REP 1 23OCT5:201 OLA2M
379GLBR- 133 REP 2 23OCT5:2010LA2M
379GLBR- 133REP3 23OCT5:2010LA2M
RSD%
379GLBR- 229 REP 1
379GLBR- 229 REP2
379GLBR- 229 REPS
31OCT10:301 OLB2M
31OCT10:301 OLB2M
31OCT10:301 OLB2M
RSD%
379GLBR- 333 REP1 19NOV5:2010LC2M
379GLBR- 333 REP 2 19NOV5:201 OLC2M
379GLBR- 333 REPS 19NOV5:2010LC2M
RSD%
379GLBR- 405 REP 1 21NOV4:359LD1M
379GLBR- 405 REP2 21NOV4:359LD1M
379GLBR- 405 REP 3 21NOV4:359LD1M
RSD%
4.15 *
4.40 *
4.15*
3%
1.76*
1.76 *
1.76 *
0%
1.64 '
1.64 *
2.14 *
16%
800
620
750
13%
0.83
0.83
0.82
1%
0.45
0.45
0.45
0%
0.12
0.11
0.12
5%
1950
1950
1950
0%
2.97*
2.97 *
3.56*
11%
1.78*
2.37 *
2.37 •
16%
13.1 *
14.2 *
14.8 *
6%
580
560
560
2%
F
F
F
F
F
F
F
F
F
* - Analyzed by Graphite Furnace AA
F - Samples were filtered prior to analysts.
U - Below detection limits
RSD % - Relative Standard Deviation.
Page 6
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN WATER SAMPLES
MSLCode
379GLBR- 127
379GLBR- 131
379GLBR- 133
379GLBR- 163
379GLBR- 170
379GLBR- 171
379GLBR- 203
379GLBR- 188
379GLBR- 189
379GLBR- 223
379GLBR- 228
379GLBR- 229
379GLBR- 251
379GLBR- 254
379GLBR- 255
379GLBR- 270
379GLBR- 274
379GLBR- 290 Rep 1
379GLBR- 290 Rep 2
379GLBR- 290 Rep 3
379GLBR- 292
379GLBR- 293
379GLBR- 328
379GLBR- 333 Rep 1
379GLBR- 333 Rep 2
379GLBR- 333 Rep 3
379GLBR- 334
379GLBR- 362
379GLBR- 363
379GLBR- 368
379GLBR- 371
379GLBR- 372
Sponsor ID
I BIN A
: 23OCT4.-459LA2M
23OCT5:2510LA2M
23OCT5:2010LA2M
25OCT1 0:201 OLA3M
25OCT11:0010LA3M
25OCT10:009LA3M
30OCT4:216LA3M
| BIN B
25OCT3:1210LB1M
25OCT3:3010LB1M
31OCT10:089LB2M
31 OCT1 0:201 OLB2M
31 OCT1 0:301 OLB2M
31OCT3:5010LB3M
31OCT2:5710LB3M
31OCT3:069LB3M
1NOV11:006LB2M
1NOV2:506LB1B3M
| BINC
18NOV5:309LC1M
18NOV5:309LC1M
18NOV5:309LC1M
18NOV6:1810LC1M
18NOV6:1810LC1M
19NOV5:559LC2M
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:3510LC2M
20NOV2.-173LC3M
20NOV2:173LC3M
20NOV2:439LC3M
20NOV3:0310LC3M
20NOV3:0710LC3M
Hg (ug/L)
CVAA
I
64.07
3.98
0.96
7.38
0.43
3.27
0.001
1.28
0.52
5.28
1.83
1.11
5.39
2.37
2.40
< 0.005
0.001
10.99
8.30
8.60
0.31
2.37
2.16
4.40
4.20
4.19
1.83
< 0.005
< 0.005
< 0.005
0.69
2.92
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN WATER SAMPLES
MSLCode Sponsor ID
.
I BIN D |
379GLBR- 399 21NOV3:3810LD1M
379GLBR- 400 21NOV3:4510LD1M
379GLBR- 405 21NOV4:359LD1M
I DILUTION WATER |
379GLBR- 277 6NOV12:003LM
Blank 1
Blank 2
Blank 3
STANDARD REFERENCE MATERIAL
SRM 1641b Rep1
SRM 16415 Rep 2
SRM 1641 b Rep 3
SRM 1641 b Rep 4
SRM 1641 b Rep5
SRM 1641 b Rep 6
SRM 1641 b Rep 7
certified
value
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-290 • 18NOV5:309LC1M
379GLBR-290 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-290 * DUPLICATE
379GLBR-290 + Spike
Amount Recovered
Percent Recovery
Hg (ug/L)
CVAA
5.25
1.48
3.20
0.003
0.017
0.021
0.047
nq/l
1.46
1.45
1.82
1.59
1.41
1.37
1.44
1.52
±0.04
5
9.30
15.68
6.38
128%
5
9.30
17.03
7.73
155%
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
MERCURY IN WATER SAMPLES
MSLCode
Sponsor ID
Hg (ug/L)
CVAA
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-334
379GLBR-334+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-334
379GLBR-334+ Spike
Amount Recovered
Percent Recovery
REPLICATE ANALYSIS
379GLBR- 290 Rep 1
379GLBR- 290 Rep 2
379GLBR- 290 Rep 3
19NOV5:3510LC2M
DUPLICATE
18NOV5:309LC1M
18NOV5:309LC1M
18NOV5:309LC1M
RSD%
5
1.83
7.58
5.76
115%
5
1.83
6.39
4.56
91%
10.99
8.30
8.60
16%
379GLBR- 333 Rep 1
379GLBR- 333 Rep 2
379GLBR- 333 Rep 3
19NOV5:2010LC2M
19NOV5:2010LC2M
19NOV5:2010LC2M
RSD%
4.40
4.20
4.19
3%
NOTE: All results are blank-corrrected.
* « Mean of replicated sample.
RSD % « Relative Standard Deviation.
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 39
379GLBR- 44
379GLBR- 45
379GLBR- 54
379GLBR- 55
379GLBR- 56
379GLBR- 98
379GLBR- 105
379GLBR- 109
379GLBR- 1 1 0
379GLBR- 1 1 4
379GLBR- 1 1 6
379GLBR- 1 1 7
379GLBR- 1 1 8
379GLBR- 134
379GLBR- 137
379GLBR- 140
379GLBR- 140
379GLBR- 140
379GLBR- 142
379GLBR- 144
379GLBR- 147
379GLBR- 148
379GLBR- 149
379GLBR- 157
379GLBR- 169
Sponsor ID
I BIN A I
070CT12:411SAS
07OCT1 2:321 SAS
07OCT12.-121SAS
09OCT11:282SA1S
09OCT11:382SA2S
09OCT11:502SA3S
22OCT11:307SA1S
22OCT11:368SA1S
22OCT4:203SA2S
22OCT5:553SA2S
23OCT1 :303SA2S
23OCT4:254SA2S
23OCT4:264SA2S
23OCT4:274SA2S
240CT10:457SA2S
24OCT10:508SA2S
Rep1 24OCT2:203SA3S
Rep 2 24OCT2:203SA3S
Rep 3 240CT2:203SA3S
240CT5:503SA3S
24OCT6:203SA3S
250CT9:234SA3S
25OCT9:244SA3S
25OCT9:254SA3S
25OCT9:307SA3S
25OCT9:358SA3S
Total Solids
(% Dry Wt.)
55.19
58.13
60.66
60.54
62.97
60.15
64.59
98.45
52.16
55.62
55.69
99.81
99.77
99.78
95.34
77.07
53.65
53.94
55.22
55.79
56.42
99.44
99.45
99.48
97.54
99.57
Total Volatile
Solids (%Dry Wt.)
6.39
6.12
6.63
5.62
5.96
6.03
6.46
4.65
5.84
5.08
5.72
3.44
3.52
3.22
4.69
2.29
5.83
5.96
6.08
5.16
5.02
4.54
3.73
4.46
5.42
4.73
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 36
379GLBR-41
379GLBR-42
379GLBR- 62
379GLBR- 63
379GLBR- 64
379GLBR- 1 72
379GLBR- 1 73
379GLBR- 1 75
379GLBR- 1 78
379GLBR- 1 79
379GLBR- 180
379GLBR- 191
379GLBR- 1 94
379GLBR- 200
379GLBR- 205
379GLBR- 209
379GLBR- 212
379GLBR- 216 Rep 1
379GLBR- 216 Rep 2
379GLBR- 216 Rep 3
379GLBR- 217
379GLBR- 218
379GLBR- 235
379GLBR- 236
379GLBR- 237
379GLBR- 238
379GLBR- 239
379GLBR- 240
379GLBR- 264
379GLBR- 266
Sponsor ID
I BIN & |
07OCT1:111SBS
07OCT1:021SBS
07OCT1 2:501 SBS
09OCT9:552SB1S
09OCT10:152SB2S
09OCT10:352SB3S
30OCT2:573SB2S
250CT12:153SB1S
25OCT2:153SB1S'
25OCT2:304SB1S
250CT2:314SB1S
25OCT2:324SB1S
25OCT3:517SB1S
25OCT3:568SB1S
30OCT4:053SB2S
30OCT4:393SB2S
310CT9:017SB2S
31OCT9:068SB2S
31OCT9:204SB2S
31OCT9:204SB2S
31OCT9:204SB2S
31OCT9:234SB2S
31OCT9:224SB2S
31OCT2:364SB3S
31OCT11:503SB3S
310CT10:453SB3S
31OCT2:303SB3S
31OCT2:374SB3S
31OCT2-.374SB3S
1NOV10.-208SB3S
1NOV10:157SB3S
Total Solids
(% Dry Wt.)
55.89
55.22
54.55
63.18
62,04
63.01
53.39
55.20
56.91
98.81
98.67
98.75
99.07
99.51
55.27
55.16
87.07
99.52
99.84
99.84
99.84
99.76
99.71
99.74
52.57
55.34
52.45
99.77
99.75
99.35
91.30
Total Volatile
Solids (%Dry Wt.)
5.94
5.90
6.62
5.72
5.58
5.61
4.99
5.28
5.80
3.42
3.41
4.22
5.08
5.00
5.73
5.67
3.83
3.79
2.17
2.81
2.91
2.04
2.96
3.90
5.73
5.80
4.68
4.03
4.41
4.39
4.95
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 37
379GLBR- 38
379GLBR-40
379GLBR- 70
379GLBR-71
379GLBR- 72
379GLBR- 279
379GLBR- 281
379GLBR- 283
379GLBR- 296
379GLBR- 297
379GLBR- 298
379GLBR- 306
379GLBR- 309
379GLBR- 310
379GLBR- 312
379GLBR-314
379GLBR-317
379GLBR-318
379GLBR- 319 Rep 1
379GLBR-319 Rep 2
379GLBR-319 Rep 3
379GLBR- 338
379GLBR- 339
379GLBR- 341
379GLBR- 343
379GLBR- 347
379GLBR- 348
379GLBR- 349
379GLBR- 355
379GLBR- 358
Sponsor ID
I BIN C. I
07OCT1-.2012SCS
07OCT1:431SCS
07OCT1:331SCS
09OCT4:362SC2S
09OCT4:552SC1S
090CT4:152SC3S
18NOV2:553SC1S
18NOV3:503SC1S
18NOV4:403SC1S
19NOV8:554SC1S
19NOV8:564SC1S
19NOV8:574SC1S
19NOV9:228SC1S
19NOV9:337SC1S
19NOV11:303SC2S
19NOV2:203SC2S
19NOV3:553SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
20NOV8:157SC2S
20NOV1 1 :443SC3S
20NOV1 :003SC3S
20NOV1:553SC3S
20NOV3:124SC3S
20NOV3:124SC3S
20NOV3:124SC3S
20NOV3:317SC3S
20NOV3:258SC3S
Total Solids
(% Dry Wt.)
54.73
64.58
60.22
63.85
63.79
64.78
46.95
54.90
54.53
99.84
99.82
99.88
98.37
82.98
49.86
50.34
52.26
99.96
99.96
100.00
99.98
99.99
95.31
50.16
47.26
47.50
94.60
95.77
95.35
85.08
99.57
Total Volatile
Solids (%Dry Wt.)
6.30
4.29
4.78
5.25
4.91
5.53
5.53
5.29
5.35
4.35
4.38
4.11
4.22
4.88
4.87
5.27
5.56
4.23
3.62
2.90
4.04
3.95
4.87
5.01
5.04
4.83
3.78
3.76
4.77
5.24
4.75
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN SEDIMENT SAMPLES
MSLCode
379GLBR- 34
379GLBR- 35
379GLBR- 43
379GLBR- 48
379GLBR- 50
379GLBR- 52 Rep 1
379GLBR- 52 Rep 2
379GLBR-52 Rep 3
379GLBR- 375
379GLBR- 377
379GLBR- 379
379GLBR- 382 Rep 1
379GLBR- 382 Rep 2
379GLBR-382 Rep 3
379GLBR- 387
379GLBR- 392
379GLBR- 393
379GLBR- 394
BLANK RESULTS
Blank 1
Blank 2
Blank 3
Blank 4
Blank 5
Blank 6
Blank 7
Blank 8
Blank 9
Blank 10
Sponsor ID
I BIN D- I
07OCT2:091SDS
07OCT1:521SDS
07OCT2:051SDS
08OCT5:312SD2S
08OCT5:412SD1S
08OCT5:172SD3S
08OCT5:172SD3S
080CT5:172SD3S
21NOV12:003SD1S
21NOV1:353SD1S
21NOV2:433SD1S
21NOV4:558SD1S
21NOV4:558SD1S
21NOV4:558SD1S
21NOV5:087SD1S
21NOV5:214SD1S
21NOV5:214SD1S
21NOV5:214SD1S
Total Solids Total Volatile
(% Dry Wt.) Solids (%Dry Wt.)
54.45
57.43
58.76
58.01
59.33
57.44
58.06
58.14
40.67
47.67
45.34
99.56
99.55
99.57
94.22
99.87
99.89
99.87
Total Solids Total
(concentrations
0.0005
0.0013
0.0001
O.OOC5
0.0006
0.0005
0.0001
0.0010
0.0014
0.0011
5.64
5.53
5.21
5.68
5.36
5.98
6.38
5.92
4.09
5.29
5.37
4.48
4.29
4.63
5.11
3.81
3.48
2.79
Volatile Solids
in grams)
0.0009
0.0017
0.0012
0.0008
0.0012
0.0001
0.0005
0.0023
0.0008
0.0025
NOTE: Results are not blank-corrected.
NA • Not applicable/analyzed.
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN SEDIMENT SAMPLES
Total Solids Total Volatile
MSLCode Sponsor ID (% Dry Wt.) Solids (%Pry Wt.)
REPLICATE ANALYSIS
379GLBR- 140 Rep 1 24OCT2:203SA3S 53.65 5.83
379GLBR- 140 Rep2 240CT2:203SA3S 53.94 5.96
379GLBR- 140 Rep 3 24OCT2:203SA3S 55.22 6.08
RSD% 2% 2%
379GLBR-216 Rep 1 31 OCT9:204SB2S 99.84 2.17
379GLBR- 216 Rep 2 31 OCT9:204SB2S 99.84 2.81
379GLBR- 216 Rep 3 310CT9:204SB2S 99.84 2.91
RSD% 0% 15%
379GLBR- 319 Rep 1 19NOV4:314SC2S 100.00 2.9
379GLBR- 319 Rep 2 19NOV4:314SC2S 99.98 4.04
379GLBR- 319 Rep 3 19NOV4:314SC2S 99.99 3.95
RSD% 0% 17%
379GLBR-52 Rep 1 08OCT5:172SD3S 57.44 5.98
379GLBR-52 Rep 2 08OCT5:172SD3S 58.06 6.38
379GLBR-52 Rep 3 08OCT5:172SD3S 58.14 5.92
RSD% 1% 4%
379GLBR- 382 Rep 1 21NOV4:558SD1S 99.56 4.48
379GLBR- 382 Rep 2 21NOV4:558SD1S 99.55 4.29
379GLBR- 382 Rep 3 21NOV4:558SD1S 99.57 4.63
RSD% 0% 4%
RSD % - Relative Standard Deviation.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
SOLIDS IN WATER SAMPLES
MSL Code
379GLBR- 95
379GLBR- 100
379GLBR- 126
379GLBR- 130 Rep 1
379GLBR- 130 Rep 2
379GLBR- 130 Rep 3
379GLBR- 158
379GLBR- 159
379GLBR- 202
379GLBR- 197 Rep 1
379GLBR- 197 Rep 2
379GLBR- 197 Rep 3
379GLBR- 224
379GLBR- 230
379GLBR- 258
379GLBR- 259
379GLBR- 260
379GLBR- 261
379GLBR- 289 Rep 1
379GLBR- 289 Rep 2
379GLBR- 289 Rep 3
379GLBR- 291
379GLBR- 329
379GLBR- 332
379GLBR- 364
379GLBR- 367
Sponsor ID
-
BIN A
21OCT:6.2410I_A1S
21OCT6:459I_A1S
23OCT4:459LA2S
23OCT5:2010LA2S
230CT5:2010LA2S
23OCT5:2010LA2S
250CT1 0:221 OLA3S
250CT10:2110LA3S
30OCT4:166LA3S
BIN B
25OCT3:1110LB1S
25OCT3:1110LB1S
25OCT3:1110LB1S
31OCT10:059LB2S
31OCT10:1910LB2S
31OCT2:5410LB3S
31OCT2:5610LB3S
31OCT3:049LB3S
31OCT3:059LB3S
BIN C
18NOV5:409LC1S
18NOV5:409LC1S
18NOV5:409LC1S
18NOV6:1010LC1S
19NOV5:539LC2S
19NOV5:2410LC2S
20NOV2:163LC3S
20NOV2:409LC3S
379GLBR- 373 20NOV3:0010LC3S
Total Solids
(mg/L)
I
4214 •
7690 *
10486 *
7824 "
8196 *
8054 *
12386 *
3564 *
184 *
7626 *
7910 *
7674 *
6768
2016
990
1156
6482
6810
11410 *
8324 *
8164 *
2172 *
4918 *
1248 *
386 *
9420 *
996 *
Total Suspended
Solids (mg/L)
318
244
344
4947
4810
5113
11080 *
2512*
23 *
7368 *
7040 *
7384 *
216
616
950
972
528
776
4748 *
5376 *
3878 *
1273 *
3184 *
863 *
<1 *
8760 *
638 *
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF0379)
SOLIDS IN WATER SAMPLES
MSLCode
379GLBR- 401
379GLBR- 403
379GLBR- 403
379GLBR- 403
Sponsor ID
-
I BIN D
21NOV3:3510LD1S
Rep1 21NOV4.-039LD1S
Rep 2 21NOV4:039LD1S
Rep 3 21NOV4:039LD1S
I DILUTION WATER
Total Solids
(ma/L)
1848
3908
3954
3970
Total Suspended
Solids (mq/L)
1156
2736
2614
2634
379GLBR- 276 6NOV12:003LS
REPLICATE ANALYSES
379GLBR- 130 Rep 1 230CT5:2010I_A2S
379GLBR- 130 Rep 2 23OCT5:2010LA2S
379GLBR- 130 Rep 3 23OCT5:2010LA2S
RSD %
379GLBR- 197 Rep 1 25OCT3:1110LB1S
379GLBR- 197 Rep 2 25OCT3:1110LB1S
379GLBR- 197 Rep 3 250CT3:1110LB1S
RSD %
379GLBR- 289 Rep 1 18NOV5:409LC1S
379GLBR-289 Rep 2 18NOV5:409LC1S
379GLBR- 289 Rep 3 18NOV5:409LC1S
379GLBR- 403 Rep 1 21NOV4:039LD1S
379GLBR- 403 Rep 2 21NOV4:039LD1S
379GLBR- 403 Rep 3 21NOV4:039LD1S
NOTE: All results are blank-corrected.
RSD% = Relative Standard Deviation.
* = Reruns outside holding times.
RSD%
RSD %
166
7824
8196
8054
2%
7626
7910
7674
2%
11410
8324
8164
20%
3908
3954
3970
1%
8
5143
5007
5310
3%
7256 *
6928 *
7272 *
3%
2580 *
2818 *
2282 *
10%
2700
2578
2598
2%
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF SEDIMENT SAMPLES
MSLCODE
MX
379GLBR- 39
379GLBR- 44
379GLBR- 45
379GLBR- 54
379GLBR- 55
379GLBR- 56
379GLBR- 98
379GLBR- 1 05
379GLBR- 109
379GLBR- 110
379GLBR- 114
379GLBR- 1 1 6
379GLBR- 1 1 7
379GLBR- 1 1 8
379GLBR- 134
379GLBR- 137
379GLBR- 140 Rep 1
379GLBR- 140 Rep 2
379GLBR- 140 Rep 3
379GLBR- 142
379GLBR- 144
379GLBR- 147
379GLBR- 148
379GLBR- 149
379GLBR- 157
379GLBR- 169
SPONSOR ID
-
I BIN A |
07OCT12:411SAS
07OCT1 2:321 SAS
070CT12:121SAS
09OCT11:282SA1S
09OCT11:382SA2S
09OCT1 1 :502SA3S
220CT11:307SA1S
22OCT11:368SA1S
22OCT4:203SA2S
22OCT5:553SA2S
23OCT1 :303SA2S
230CT4:254SA2S
23OCT4:264SA2S
23OCT4:274SA2S
24OCT10:457SA2S
24OCT10:508SA2S
24OCT2:203SA3S
24OCT2:203SA3S
24OCT2:203SA3S
24AOCT5:503SA3S
24OCT6:203SA3S
250CT9:234SA3S
25OCT9:244SA3S
25OCT9:254SA3S
250CT9.-307SA3S
25OCT9:358SA3S
TOC
% Dry Weight
300 ug/g
1.91
1.77
1.91
1.86
1.84
1.90
2.73
1.86
1.87
1.86
1.89
1.25
1.18
1.21
1.48
1.04
1.86
1.99
1.85
1.90
1.82
1.40
1.47
1.54
1.72
1.47
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOO ANALYSIS OF SEDIMENT SAMPLES
MSLCODE
MDL
379GLBR- 36
379GLBR- 41
379GLBR- 42
379GLBR- 62
379GLBR- 63
379GLBR- 64
379GLBR- 172
379GLBR- 173
379GLBR- 175
379GLBR- 178
379GLBR- 179
379GLBR- 180
379GLBR- 191
379GLBR- 1 94
379GLBR- 200
379GLBR- 205
379GLBR- 209
379GLBR- 212
379GLBR- 216 Rep 1
379GLBR- 216 Rep 2
379GLBR- 216 Rep 3
379GLBR- 217
379GLBR- 218
379GLBR- 235
379GLBR- 236
379GLBR- 237
379GLBR- 238
379GLBR- 239
379GLBR- 240
379GLBR- 264
379GLBR- 266
SPONSOR ID
*
| BIN B |
07OCT1:111SBS
07OCT1:021SBS
07OCT1 2:501 SBS
090CT9:552SB1S
09OCT10:152SB2S
09OCT10:352SB3S
300CT2.-573SB2S
25OCT12.-153SB1S
25OCT2:153SB1S
25OCT2:304SB1S
25OCT2:314SB1S
25OCT2:324SB1S
250CT3:517SB1S
25OCT3:568SB1S
30OCT4:053SB2S
30OCT4:393SB2S
31OCT9:017SB2S
31OCT9:068SB2S
31OCT9:204SB2S
31OCT9:204SB2S
31OCT9:204SB2S
31OCT9:234SB2S
31OCT9:224SB2S
31OCT2:364SB3S
31OCT11:503SB3S
31OCT10-.453SB3S
31OCT2:303SB3S
31OCT2:374SB3S
31OCT2:374SB3S
1NOV10:208SB3S
1NOV10:157SB3S
TOC
% Dry Weight
300 ug/g
1.93
1.67
1.91
1.82
1.87
1.94
2.14
1.94
1.84
1.49
1.40
1.37
1.71
1.69
1.81
1.79
1.59
1.53
0.99
1.02
1.13
1.02
1.01
1.52
1.80
2.01
1.78
1.39
1.39
1.46
1.42
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF SEDIMENT SAMPLES
MSLCODE
MX
379GLBR- 37
379GLBR- 38
379GLBR- 40
379GLBR- 70
379GLBR- 71
379GLBR- 72
379GLBR- 279
379GLBR- 281
379GLBR- 283
379GLBR- 296
379GLBR- 297
379GLBR- 298
379GLBR- 306
379GLBR- 309
379GLBR- 310
379GLBR- 312
379GLBR- 314
379GLBR- 317
379GLBR- 318
379GLBR- 319 Rep 1
379GLBR- 319 Rep 2
379GLBR- 319 Rep 3
379GLBR- 338
379GLBR- 339
379GLBR- 341
379GLBR- 343
379GLBR- 347
379GLBR- 348
379GLBR- 349
379GLBR- 355
379GLBR- 358
SPONSOR ID
*
I BIN C I
07OCT1:201SCS
07OCT1:431SCS
07OCT1:331SCS
09OCT4:362SC2S
09OCT4:552SC1S
09OCT4:152SC3S
18NOV2:553SC1S
18NOV3:503SC1S
18NOV4:403SC1S
19NOV8:554SC1S
19NOV8.-564SC1S
19NOV8:574SC1S
19NOV9:228SC1S
19NOV9:337SC1S
19NOV11:303SC2S
19NOV2:203SC2S
19NOV3:553SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
19NOV4:314SC2S
20NOV8:157SC2S
20NOV11:443SC3S
20NOV1:003SC3S
20NOV1:553SC3S
20NOV3:124SC3S
20NOV3:124SC3S
20NOV3:124SC3S
20NOV3:317SC3S
20NOV3:258SC3S
TOC
% Dry Weight
300 ug/g
1.80
1.62
1.89
1.77
1.80
1.84
1.84
1.82
1.83
1.49
1.47
1.61
1.46
2.06
1.78
1.85
1.78
1.49
1.57
1.49
1.59
1.56
1.66
1.76
1.76
1.73
1.67
1.61
1.70
2.05
1.59
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF SEDIMENT SAMPLES
MSLCODE
MX
379GLBR- 34
379GLBR- 35
379GLBR- 43
379GLBR- 48
379GLBR- 50
379GLBR- 52 Rep 1
379GLBR- 52 Rep 2
379GLBR- 52 Rep 3
379GLBR- 375
379GLBR- 377
379GLBR- 379
379GLBR- 382 Rep 1
379GLBR- 382 Rep 2
379GLBR- 382 Rep 3
379GLBR- 387
379GLBR- 392
379GLBR- 393
379GLBR- 394
BLANK Rep 1
BLANK Rep 2
BLANK Rep 3
BLANK Rep 4
BLANK Rep 5
BLANK Rep 6
BLANK Rep 7
BLANK Rep 8
BLANK Rep 9
BLANK Rep 10
SPONSOR ID
I BIN D |
07OCT2:091SDS
07OCT1:521SDS
07OCT2:051SDS
08OCT5:312SD2S
080CT5:412SD1S
08OCT5:172SD3S
08OCT5:172SD3S
08OCT5:172SD3S
21NOV12:003SD1S
21NOV1:353SD1S
21NOV2:433SD1S
21NOV4:558SD1S
21NOV4:558SD1S
21NOV4:558SD1S
21NOV5:087SD1S
21NOV5:214SD1S
21NOV5:214SD1S
21NOV5:214SD1S
TOC
% Dry Weight
300 ug/g
1.78
1.76
1.74
2.55
1.82
1.91
1.98
1.91
1.85
1.84
1.85
1.53
1.53
1.53
1.84
1.35
1.26
1.36
0.006
0.005
0.005
0.005
0.003
0.005
0.003
0.004
0.005
0.003
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF SEDIMENT SAMPLES
MSLCODE
MDL
SPONSOR ID
TOC
% Dry Weight
300 ug/g
STANDARD REFERENCE MATERIAL
MESS-1
MESS-1
MESS-1
MESS-1
MESS-1
Rep 1
Rep 2
Rep 3
Rep 4
Rep 5
certified
value
2.42
2.41
2.37
2.39
2.25
2.25
±0.2
REPLICATE ANALYSES
379GLBR- 140
379GLBR- 140
379GLBR- 140
379GLBR- 216
379GLBR- 216
379GLBR- 216
379GLBR- 319
379GLBR- 319
379GLBR- 319
379GLBR-
379GLBR-
379GLBR-
52
52
52
379GLBR- 382
379GLBR- 382
379GLBR- 382
Rep 1 24OCT2:203SA3S
Rep 2 24OCT2:203SA3S
Rep 3 24OCT2:203SA3S
Rep1 31OCT9:204SB2S
Rep 2 31OCT9:204SB2S
Rep 3 31OCT9:204SB2S
Rep1 19NOV4:314SC2S
Rep 2 19NOV4:314SC2S
Rep 3 19NOV4:314SC2S
Rep 1 08OCT5:172SD3S
Rep 2 08OCT5:172SD3S
Rep 3 08OCT5:172SD3S
Rep 1 21NOV4:558SD1S
Rep 2 21 NOV4:558SD1 S
Rep 3 21NOV4:558SD1S
RSD %
RSD %
RSD %
RSD %
RSD %
1.86
1.99
1.85
4%
0.99
1.02
1.13
7%
1.49
1.59
1.56
3%
1.91
1.98
1.91
2%
1.53
1.53
1.53
0%
NOTE: Results are blank-corrected.
RSD % - Relative Standard Deviation.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOO ANALYSIS OF WATER SAMPLES
MSLCODE
ACt
379GLBR- 125
379GLBR- 129
379GLBR- 162
379GLBR- 165
379GLBR- 201
379GLBR- 190
379GLBR- 225
379GLBR- 231
379GLBR- 262
379GLBR- 263
379GLBR- 271
379GLBR- 273
379GLBR- 294
379GLBR- 295
379GLBR- 330
379GLBR- 335
379GLBR- 365
379GLBR- 369
379GLBR- 374
379GLBR- 402
379GLBR- 406
379GLBR- 278
3LANK Rep 1
3LANK Rep 2
3LANK Rep 3
SPONSOR ID
I BIN A I
23OCT4:459LA2C
23OCT5:2010LA2C
25OCT10:2110LA3C
25OCT10:009LA3C
30OCT4:206LA3C
I BIN B I
25OCT3:1110LB1C
310CT10:109LB2C
31 OCT1 0:241 OLB2C
31OCT2:5810LB3C
310CT3:099LB3C
1NOV11:006LB2C
1NOV2:506LB1B3C
I BIN C I
18NOV6:0610LC1C
18NOV5:459LC1C
19NOV5:579LC2C
19NOV5:4310LC2C
20NOV2:183LC3C
20NOV2:449LC3C
20NOV3:0210LC3C
I BIN D |
21NOV3:3710LD1C
21NOV4:459LD1C
| DILUTION WATER |
6NOV12:003LC
TOG
(UO/L)
1000 ug/L
2392600
853490
509150
716190
530
531430
854650
747090
437250
909520
350
400
275150
829720
715150
251420
7120
428120
167150
373020
695120
1370
< 990
< 810
< 360
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF WATER SAMPLES
MSLCODE
MDL
SPONSOR ID
TOC
(ug/L)
1000 ug/L
REPLICATE ANALYSES
379GLBR- 263 Rep 1
379GLBR- 263 Rep 2
379GLBR- 263 Rep 3
379GLBR- 295 Rep 1
379GLBR- 295 Rep 2
379GLBR- 295 Rep 3
379GLBR- 335 Rep 1
379GLBR- 335 Rep 2
379GLBR- 335 Rep 3
379GLBR- 278 Rep 1
379GLBR- 278 Rep 2
379GLBR- 278 Rep 3
31OCT3:099LB3C
310CT3:099LB3C
31OCT3:099LB3C
18NOV5:459LC1C
18NOV5:459LC1C
18NOV5:459LC1C
19NOV5:4310LC2C
19NOV5:4310LC2C
19NOV5:4310LC2C
6NOV12:003LC
6NOV12:003LC
6NOV12:003LC
RSD%
RSD %
RSD%
RSD%
902000
935000
905000
2%
829720
850280
856480
2%
251420
240650
238680
3%
1370
1390
1390
1%
NOTE: Results are blank-corrected.
RSD % * Relative Standard Deviation.
Page 2
-------
REPORT OF CHEMICAL ANALYSES
Volume 2: Leach Test
PROJECT: Buffalo River Pilot Project
Prepared for:
USEPA Great Lakes National Program Office
Attn: Dr. Steve Garbaciak
230 S. Dearborn
Chicago, IL 60604
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: BUFFALO RIVER PILOT PROJECT
ISSUED TO: Dr. Steve Garbaciak
Technical Project Manager
USEPA Great Lakes National Program Office
230 S. Dearborn
Chicago, IL 60604
INTRODUCTION
DATE: April 23, 1992
CF#: 379GLBR
This report summarizes the results from analyses performed on pilot study samples which
were submitted by the U.S. Army Corps of Engineers Great Lakes Division, Buffalo District.
SAMPLE CUSTODY
Samples were received in good condition from October 7, 1991 through December 5, 1991.
Samples were logged in and stored as specified in the narrative. Samples were analyzed
within the holding times specified in the QA plan. Any exceptions are noted in the narrative
associated with each analysis.
LEACH TEST AND TCLP EXTRACTIONS
Twenty-one samples were leached following the sequential batch leach test (SBLT) and the
toxicity characteristic leaching procedure (TCLP) provided by the Army Corps of Engineers-
Buffalo District. All leach test samples were stored at 4°±2<>C prior to leaching. The SBLT
produced four extracts for each sample which were subsampled for each parameter, then
analyzed separately for metals, specific conductivity, TOC and pH. Metal and TOC aliquots
were acidified upon collection to a pH £.2 with nitric acid and phosphoric acid, respectively.
Specific conductivity aliquots were stored at 4°±2°C until analysis. pH was determined
immediately and the aliquots were archived at 4°±2°C. The TCLP produces one extract for
each sample which was then analyzed for metals and pH. The metals aliquot was acidified to
a pH sSL upon collection. pH was determined immediately and the aliquot archived at 4°±2<>C.
Twelve samples were archived for possible analysis in the future. Samples for TOC were
sent to Analytical Resources, Inc. for analysis by EPA method 415.1 and measured on a
Dohrman DC-180 Organic Carbon Analyzer. Specific conductance and pH were determined
potentiometrically, following Standard Methods 2510 B and EPA method 150.1, respectively.
Cadmium, chromium and lead were analyzed by stabilized temperature graphite furnace,
following Battelle SOP# MSL-M-32. Mercury was analyzed by cold vapor atomic
fluorescence, following Battelle SOP# MSL-M-27.
Sponsor ID
07OCT12:381 SAL
07OCT12:571 SBL
07OCT12:301 SAL
0?OCT1:071SBL
23OCT4:354SA2M
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Battelle ID
379GLBR*5
379GLBR*7
379GLBR*8
379GLBR*10
379GLBR*121
-------
25OCT9:104SA3M
25OCT2:514SB1M
31OCT9:304SB2M
31OCT2:404SB3M
4DEC11:455SA2M
4DEC11:555SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC11:305SA3M
4DEC11:375SA3M
4DEC12:505SB2M
4DEC1.-005SB2M
4DEC1:155SB2M
4DEC1:255SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
379GLBRM54
379GLBFT185
379GLBFT214
379GLBFT250
379GLBFV460
379GLBRM61
379GLBRM62
379GLBRM63
379GLBRM64*
379GLBRM65*
379GLBRM66
379GLBRM67*
379GLBR*468*
379GLBRM69
379GLBRM70*
379GLBRM71*
Leach Test
*The second, third and fourth extracts of these leach test were not analyzed, but archived
for possible future analysis as directed by the Army Corps of Engineers-Buffalo District.
ARCHIVED SAMPLES
Sponsor ID
07OCT1:451SCL
07OCT1.-501SDL
07OCT2:061SDL
07OCT2:151SDL
07OCT1:401SCL
07OCT1.-141SBL
07OCT1:261SCL
07OCT12:451 SAL
21OCT5:504SA1L
19NOV8:504SC1M
19NOV4:374SC2M
20NOV3:204SC3M
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Leach Test
Battelle ID
379GLBR"!
379GLBR*2
379GLBR*3
379GLBRM
379GLBR*6
379GLBR*9
379GLBR*11
379GLBRM2
379GLBR*87
379GLBR*301
379GLBR*322
379GLBR*354
Metals
The SBLT samples could not be spiked for metals prior to extraction as at a pH >2, metals
tend to remain in the sediment. Therefore, any matrix spike added would adsorb onto the
sediment and recoveries would be meaningless. Although two TCLP samples (379GLBR*5 and
465) were spiked with 40 jig of Pb, 20 u.g of Cu and 20 ng of Cr prior to extraction, the pH in
the extraction fluid was ~ 5, consequently, the metal spikes were not recovered. The
analyst performed spike additions at the time of analysis for both the SBLT and TCLP
samples. Since spike additions are not true matrix spikes, that data is not presented on the
final summary tables but is available in the raw data. Replicate analyses were quite
variable for the metals analysis of both TCLP and SBLT extracts, which may be due in part
to nonhomogeneous samples and partly to values near the method detection limits.
Variability increased for the treated sediment (ash) samples and may be a result of matrix
interference. Certified reference material values were always within the ARCS criteria of ±
20%.
-------
Replicates of the leaching procedure for TOO produced variable results, of which some were
outside the ARCS criteria. Replicates performed at the time of analysis produced RSD values
within the ARCS criteria, indicating the variability comes from the leach procedure itself,
rather than the TOC methodology. Generally, the first fraction results were consistent with
an RSD - 15%, suggesting the variability in extraction efficiency lies in the following days
of the method. Variability increased for the treated sediment (ash) samples and may be a
result of matrix interference.
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
379GLBR- 5
379GLBR- 5
379GLBR- 5
379GLBR- 8
379GLBR-121
379GLBR-121
379GLBR-121
379GLBR- 1 54
^
;
Rep 1 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Rep 2 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Rep 3 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Rep 1 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Rep 2 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Rep 3 Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
I BIN A |
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
pH
7.74
7.83
7.93
7.99
7.75
7.93
8.06
7.97
7.63
7.93
8.05
8.01
6.80
7.20
7.56
7.89
7.66
7.63
7.82
7.80
7.57
7.87
7.68
7.80
7.69
7.84
7.77
7.83
7.38
7.51
7.82
8.04
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
379GLBR-460
379GLBR-461
379GLBR- 462
379GLBR-463
379GLBR-464
379GLBR-465
379GLBR- 7
379GLBR- 10
379GLBR-214
379GLBR- 250
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
4DEC11:455SA2M
4DEC11:455SA2M
4DEC1 1 :455SA2M
4DEC1 1 :455SA2M
4DEC1 1 :555SA2M
4DEC11 :555SA2M
4DEC1 1 :555SA2M
4DEC11:555SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC1 1 :305SA3M
4DEC11:375SA3M
I BIN B |
070CT1 2:571 SBL
07OCT1 2:571 SBL
07OCT1 2:571 SBL
07OCT1 2:571 SBL
07OCT1:071SBL
07OCT1:071SBL
07OCT1:071SBL
07OCT1:071SBL
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9:304SB2M
310CT2:404SB3M
31OCT2:404SB3M
31OCT2:404SB3M
310CT2:404SB3M
PH
12.05
12.38
12.27
11.80
12.01
12.42
12.32
11.95
12.08
12.40
12.31
11.98
12.45
12.50
11.02
11.03
12.28
12.26
7.47
7.79
7.80
7.68
7.92
7.84
7.78
7.79
7.34
7.73
7.96
8.06
7.32
7.53
7.72
7.82
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
379GLBR-466
379GLBR-467
379GLBR-468
379GLBR-469
379GLBR-470
379GLBR-471
BLANK-1
BLANK-1
BLANK-1
BLANK-1
BLANK-2
BLANK-2
BLANK-2
BLANK-2
BLANK-3
BLANK-3
BLANK-3
BLANK-3
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
4DEC12:505SB2M
4DEC12:505SB2M
4DEC12:505SB2M
4DEC12:505SB2M
4DEC1:005SB2M
4DEC1:155SB2M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
PH
12.19
12.48
12.44
12.27
12.32
12.30
11.93
12.20
12.08
11.98
12.42
12.43
5.60
5.75
5.63
6.00
6.85
6.25
5.04
5.18
5.32
4.89
5.07
5.57
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Sponsor ID
PH
REPLICATE ANALYSIS
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 1
5 Rep 2 Fraction 1
5 Rep 3 Fraction 1
07OCT12:381 SAL
07OCT12:381 SAL
07OCT12:381 SAL
RSD%
7.74
7.75
7.63
1%
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 2
5 Rep 2 Fraction 2
5 Rep 3 Fraction 2
07OCT12:381 SAL
07OCT12:381 SAL
07OCT12:381 SAL
RSD%
7.83
7.93
7.93
1%
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 3
5 Rep 2 Fraction 3
5 Rep 3 Fraction 3
07OCT12:381 SAL
07OCT12:381 SAL
07OCT12:381 SAL
RSD%
7.93
8.06
8.05
1%
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 4
5 Rep 2 Fraction 4
5 Rep 3 Fraction 4
379GLBR-121 Rep 1 Fraction 1
379GLBR-121 Rep 2 Fraction 1
379GLBR-121 Rep 3 Fraction 1
379GLBR-121 Rep 1 Fraction 2
379GLBR-121 Rep 2 Fraction 2
379GLBR-121 Rep 3 Fraction 2
07OCT12:381 SAL
07OCT12:381 SAL
07OCT12:381 SAL
RSD%
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
RSD%
23OCT4:354SA2M
23OCT4.-354SA2M
23OCT4:354SA2M
RSD%
7.99
7.97
8.01
0%
7.66
7.57
7.69
1%
7.63
7.87
7.84
2%
RSD % « Relative Standard Deviation.
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode Sponsor ID pH
REPLICATE ANALYSIS
379GLBR-121 Rep 1 Fraction 3 23OCT4:354SA2M 7.82
379GLBR-121 Rep 2 Fraction 3 23OCT4:354SA2M 7.68
379GLBR-121 Rep 3 Fraction 3 230CT4:354SA2M 7.77
RSD% 1%
379GLBR-121 Rep 1 Fraction 4 23OCT4:354SA2M 7.80
379GLBR-121 Rep 2 Fraction 4 23OCT4:354SA2M 7.80
379GLBR-121 Rep 3 Fraction 4 23OCT4:354SA2M 7.83
RSD % 0%
RSD % - Relative Standard Deviation.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(TCLP EXTRACTONS)
MSLCode
379G'.BR- 5 Rep 1
379GLBR- 5 Rep 2
379GLBR- 5 Rep 3
379GLBR- 8
379GLBR- 121 Rep 1
379GLBR- 121 Rep 2
379GLBR- 121 Rep 3
379GLBR- 1 54
379GLBR- 460
379GLBR- 461
379GLBR- 462
379GLBR- 463
379GLBR- 464
379GLBR- 465
379GLBR- 7
379GLBR- 1 0
379GLBR- 214
379GLBR- 250
379GLBR- 466
379GLBR- 467
379GLBR- 468
379GLBR- 469
379GLBR- 470
379GLBR- 471
BLANK-1
BLANK-2
Sponsor ID
I BIN A |
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:301 SAL
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
25OCT9:104SA3M
4DEC1 1 :455SA2M
4DEC1 1 :555SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC1 1 :305SA3M
4DEC11:375SA3M
I BIN B |
07OCT1 2:571 SBL
07OCT1:071SBL
31OCT9:304SB2M
31OCT2:404SB3M
4DEC12:505SB2M
4DEC1:005SB2M
4DEC1:155SB2M
4DEC1:255SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
PH
5.53
5.54
5.56
5.55
6.24
6.22
6.17
6.10
11.71
11.84
9.28
11.64
11.71
11.67
5.53
5.58
6.23
6.10
12.07
12.05
12.05
6.64
6.55
6.64
4.92
2.86
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
pH ANALYSIS OF LEACHATE SAMPLES
(TCLP EXTRACTONS)
MSLCode Sponsor ID pH
REPLICATE ANALYSIS
379GLBR- 5 Rep 1 07OCT 12:381 SAL 5.53
379GLBR- 5 Rep 2 07OCT12:381 SAL 5.54
379GLBR- 5 Rep 3 07OCT12:381 SAL 5.56
RSD% 0%
379GLBR- 121 Rep 1 23OCT4:354SA2M 6.24
379GLBR- 121 Rep 2 23OCT4:354SA2M 6.22
379GLBR- 121 Rep 3 23OCT4:354SA2M 6.17
RSD% 1%
RSD % - Relative Standard Deviation.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
SPECIFIC CONDUCTANCE IN LEACHATE SAMPLES
MSLCode
379GLBR-5, Rep 1
379GLBR-5, Rep 2
379GLBR-5, Rep 3
379GLBR-8
379GLBR-121, Rep 1
379GLBR-121, Rep 2
379GLBR-121, Rep 3
379GLBR-154
379GLBR-460
Fraction No.
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
| BIN A |
070CT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
070CT1 2:381 SAL
070CT1 2:381 SAL
070CT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
070CT1 2:381 SAL
070CT1 2:381 SAL
07OCT1 2:301 SAL
070CT1 2:301 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
230CT4:354SA2M
230CT4:354SA2M
23OCT4:354SA2M
230CT4:354SA2M
23OCT4.-354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
230CT4:354SA2M
23OCT4:354SA2M
23OCT4.-354SA2M
23OCT4.-354SA2M
23OCT4:354SA2M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
250CT9:104SA3M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
Specific
Conductance
(umhos/cm)
440
230
162
136
450
220
164
136
480
230
171
134
740
570
340
240
1030
230
103
89
1010
230
109
88
980
220
104
87
750
310
210
154
6960
7080
5400
4160
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
SPECIRC CONDUCTANCE IN LEACHATE SAMPLES
MSLCode
379GLBR-461
379GLBR-462
379GLBR-463
379GLBR-464
379GLBR-465
379GLBR-7
379GLBR-214
379GLBR-466
379GLBR-467
379GLBR-468
379GLBR-469
379GLBR-470
379GLBR-471
Fraction No.
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Sponsor ID
I BIN A |
4DEC1 1 :555SA2M
4DEC11:555SA2M
4DEC11:555SA2M
4DEC11:555SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:305SA3M
4DEC11:375SA3M
| BIN B |
07OCT1:571SBL
07OCT1:571SBL
07OCT1:571SBL
07OCT1:571SBL
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9:304SB2M
4DEC12:505SB2M
4DEC12:505SB2M
4DEC12:505SB2M
4DEC12:505SB2M
4DEC1:005SB2M
4DEC1:155SB2M
4DEC1:2555SB1/B3M
4DEC1:2555SB1/B3M
4DEC1:2555SB1/B3M
4DEC1:2555SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
Specific
Conductance
(umhos/cm)
7560
6960
6240
4560
7480
6840
5640
3960
9040
8720
8880
8160
9600
9680
480
230
174
200
1100
250
116
88
10160
8720
8080
8000
10240
11280
6600
5400
3320
2740
6720
7400
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
SPECIHC CONDUCTANCE IN LEACHATE SAMPLES
MSLCode
BLANK 1
BLANK 1
BLANK 1
BLANK 1
BLANK 2
BLANK 2
BLANK 2
BLANK 2
BLANKS
BLANK 3
BLANKS
BLANKS
Fraction No. - Sponsor ID
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Specific
Conductance
(umhos/cm)
3
4
2
2
3
3
8
5
13
7
5
7
STANDARD - KC2 (umhos/cm)
.01M Rep 1
.01M Rep 2
.01M Rep 3
.01M Rep 4
TRUE
VALUE
STANDARD - KC1 (umhos/cm)
.005M
.005M
.005M
.005M
Rep 1
Rep 2
Rep 3
Rep 4
TRUE
VALUE
REPLICATE ANALYSIS
379GLBR-5, Rep 1
379GLBR-5, Rep 2
379GLBR-5, Rep 3
Fraction 1
Fraction 1
Fraction 1
070CT12:381 SAL
07OCT12:381 SAL
07OCT12:381 SAL
RSD%
1410
1410
1410
1410
1413
730
730
730
730
717.8
440
450
480
5%
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
SPECIFIC CONDUCTANCE IN LEACHATE SAMPLES
MSLCode
Fraction No.
REPLICATE ANALYSIS
379GLBR-5, Rep 1
379GLBR-5, Rep 2
379GLBR-5, Rep 3
379GLBR-5, Rep 1
379GLBR-5, Rep 2
379GLBR-5, Rep 3
379GLBR-5, Rep 1
379GLBR-5, Rep 2
379GLBR-5, Rep 3
379GLBR-121, Rep 1
379GLBR-121, Rep 2
379GLBR-121, Rep 3
379GLBR-121. Rep 1
379GLBR-121, Rep 2
379GLBR-121, Rep 3
379GLBR-121, Rep 1
379GLBR-121, Rep 2
379GLBR-121, Rep 3
379GLBR-121, Rep 1
379GLBR-121, Rep 2
379GLBR-121, Rep 3
Fraction 2
Fraction 2
Fraction 2
Fraction 3
Fraction 3
Fraction 3
Fraction 4
Fraction 4
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 2
Fraction 2
Fraction 3
Fraction 3
Fraction 3
Fraction 4
Fraction 4
Fraction 4
Sponsor ID
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
RSD%
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:301 SAL
RSD%
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:301 SAL
RSD%
23OCT4.-354SA2M
230CT4:354SA2M
23OCT4:354SA2M
RSD%
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
RSD%
23OCT4:354SA2M
23OCT4.-354SA2M
23OCT4:354SA2M
RSD%
23OCT4:354SA2M
23OCT4:354SA2M
230CT4:354SA2M
RSD %
Specific
Conductance
(umhos/cm)
230
220
230
3%
162
164
171
3%
136
136
134
1%
1030
1010
980
2%
230
230
220
3%
103
109
104
3%
89
88
87
1%
RSD % = Relative Standard Deviation.
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF4379)
TOC ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Method Detection Limit
379GLBR- 5 Rep 1
379GLBR- 5 Rep 2
379GLBR- 5 Rep 3
379GLBR- 8
379GLBR- 121 Rep 1
379GLBR-121 Rep 2
379GLBR- 121 Rep 3
379GLBR- 1 54
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
I BIN A |
07OCT1 2:381 SAL
07OCT1 2581 SAL
07OCT1 2581 SAL
07OCT1 2381 SAL
07OCT1 2581 SAL
07OCT1 2581 SAL
07OCT1 2581 SAL
07OCT1 2581 SAL
07OCT1 2581 SAL
070CT1 2:381 SAL
070CT1 2581 SAL
07OCT1 2581 SAL
07OCT1 2501 SAL
070CT1 2501 SAL
07OCT1 2501 SAL
07OCT1 2501 SAL
23OCT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
230CT4554SA2M
23OCT4554SA2M
230CT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
23OCT4554SA2M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
TOC
ug/L
660
10,620
10.230
7,160
5,710
10,880
7,760
6,310
4,170
13,370
8,940
10,300
5,010
17,350
1 1 ,720
12,070
4,680
34.150
15,660
3,560
12.510
35,460
7.160
4,410
3.690
36,550
14.150
7,040
4.440
136.290
32.760
20,400
12,860
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Method Detection
379GLBR- 460
379GLBR-461
379GLBR- 462
379GLBR- 463
379GLBR- 464
379GLBR- 465
379GLBR- 7
379GLBR- 1 0
379GLBR-214
Limit
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
I BIN A |
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11355SA2M
4DEC11555SA2M
4DEC11:555SA2M
4DEC11555SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11:155SA3M
4DEC11305SA3M
4DEC11575SA3M
I BIN B |
07OCT1 2:571 SBL
07OCT1 2:571 SBL
07OCT1 2:571 SBL
07OCT1 2571 SBL
07OCT1:071SBL
070CT1:071SBL
07OCT1:071SBL
070CT1:071SBL
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9:304SB2M
31OCT9.-304SB2M
TOC
UQ/L
660
65,200
34,300
24,600
26,600
70.170
33,730
23.660
18.260
105.720
156.100
157.190
100,540
71.100
64.900
75.090
62,430
56,320
51,960
15,830
4,910
1,720
1,740
11,680
7,120
5,900
5,450
15,400
13,8X)0
3,960
3,360
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Method Detection
379GLBR- 250
379GLBR- 466
379GLBR- 467
379GLBR- 468
379GLBR- 469
379GLBR- 470
379GLBR- 471
BLANK-1
BLANK-1
BLANK-1
BLANK-1
BLANK-2
BLANK-2
BLANK-2
3LANK-2
3LANK-3
3LANK-3
3LANK-3
3LANK-3
Limit
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 1
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Sponsor ID
I BIN B |
31OCT2:404SB3M
31OCT2:404SB3M
310CT2:404SB3M
31OCT2:404SB3M
4DEC12505SB2M
4DEC12505SB2M
4DEC12505SB2M
4DEC12S05SB2M
4DEC1.-005SB2M
4DEC1:155SB2M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:255SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
TOC
ug/L
660
158,670
52,600
21,510
13,410
108.010
134,310
121,990
97.850
67.120
52,820
88.910
38,470
26,910
23,370
118,120
91,590
6,680
950
1,250
3,890
5,980
5,010
2,010
840
9.460
1,750
1,310
1,720
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
TOC ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Method Detection Limit
Sponsor ID
TOC
ug/L
660
REPLICATE ANALYSIS
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 1
5 Rep 2 Fraction 1
5 Rep 3 Fraction 1
5 Rep 1 Fraction 2
5 Rep 2 Fraction 2
5 Rep 3 Fraction 2
5 Rep 1 Fraction 3
5 Rep 2 Fraction 3
5 Rep 3 Fraction 3
07OCT12:381 SAL
07OCT12:381 SAL
07OCT12381 SAL
RSD%
07OCT12381 SAL
07OCT12381 SAL
07OCT12381 SAL
RSD%
07OCT12381 SAL
07OCT12381SAL
07OCT12381 SAL
RSD%
10,620
10,680
13,370
13%
10,230
7,760
8,940
14%
7,160
6,310
10,300
27%
379GLBR-
379GLBR-
379GLBR-
5 Rep 1 Fraction 4
5 Rep 2 Fraction 4
5 Rep 3 Fraction 4
379GLBR-121 Rep 1 Fraction 1
379GLBR-121 Rep 2 Fraction 1
379GLBR-121 Rep 3 Fraction 1
379GLBR-121 Rep 1 Fraction 2
379GLBR- 121 Rep 2 Fraction 2
379GLBR- 121 Rep 3 Fraction 2
07OCT12381 SAL
07OCT12381 SAL
07OCT12381 SAL
RSD%
23OCT4354SA2M
23OCT4354SA2M
23OCT4354SA2M
RSD%
23OCT4354SA2M
23OCT4354SA2M
23OCT4354SA2M
RSD%
5,710
4,170
5,010
16%
34,150
35,460
36,550
3%
15,660
7,160
14,150
37%
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF0379)
TOC ANALYSIS OF LEACHATE SAMPLES
(SBLT EXTRACTONS)
MSLCode
Sponsor ID
TOC
ug/L
Method Detection Limit
660
REPLICATE ANALYSIS
379GLBR-121 Rep 1 Fraction 3
379GLBR-121 Rep 2 Fraction 3
379GLBR- 121 Rep 3 Fraction 3
379GLBR-121 Rep 1 Fraction 4
379GLBR- 121 Rep 2 Fraction 4
379GLBR-121 Rep 3 Fraction 4
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4C354SA2M
RSD%
23OCT4:354SA2M
23OCT4.-354SA2M
23OCT4354SA2M
RSD%
3,560
4,410
7,040
36%
12,510
3,690
4,440
71%
RSD % - Relative Standard Deviation.
NOTE: All results are blank-corrected.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(TCLP SEDIMENT EXTRACTIONS)
MSLCode
Method Detection Limits
Sponsor ID
Cr (ug/L)
AA
0.05
Cu (ug/L)
AA
0.85
Hg (ug/L)
CVAF
_
Pb (ug/L)
AA
_
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
379GLBR-
BLANK-1
BLANK-2
5 Rep 1
5 Rep 2
5 Rep 3
8
121 Rep1
121 Rep 2
121 Rep 3
154
460
461
462
463
464
465
7
10
214
250
466
467
468
469
470
471
I BIN A j
07OCT12:381SAL
07OCT12:381SAL
07OCT1 2:381 SAL
07OCT12:301SAL
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
25OCT9:104SA3M
4DEC1 1 :455SA2M
4DEC1 1 :555SA2M
4DEC12:055SA2M
4DEC11:155SA3M
4DEC11:305SA3M
4DEC11:375SA3M
I BIN B |
07OCT1 2:571 SBL
07OCT1:071SBL
31OCT9:304SB2M
31OCT2:404SB3M
4DEC12:505SB2M
4DEC1:005SB2M
4DEC1:155SB2M
4DEC1:255SB1/B3M
4DEC1:305SB1/B3M
4DEC1:355SB1/B3M
0.40
0.36
0.36
0.62
0.22
0.22
0.36
0.71
42.37
36.40
30.77
50.39
45.62
37.13
0.76
0.62
0.13
0.71
18.04
17.50
18.04
1.91
2.29
1.82
0.09
0.09
13.6
11.2
11.7
11.2
5.3
4.4
2.9
15.1
47.6
40.8
38.4
12.6
11.2
12.1
11.2
12.1
2.4
13.6
11.7
13.1
14.6
31.6
29.6
31.1
1.9
1.0
0.00216
0.00094 U
0.00094 U
0.00094 U
0.00047 U
0.00047 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00047 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00094 U
0.00996
0.00589
0.00695
0.00094 U
0.00094 U
21.95
19.88
17.39
16.15
3.08
3.08
1.54
6.55
0.72 U
0.72 U
0.69 U
0.69 U
0.69 U
0.69 U
16.57
19.47
1.93
6.16
0.69 U
0.80
0.69 U
1.20
1.20
0.80
0.72 U
0.72 U
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(TCLP SEDIMENT EXTRACTIONS)
MSLCode
Method Detection Limits
Cr (ug/L)
Sponsor ID AA
0.05
Cu (ug/L)
AA
0.85
Hg (ug/L)
CVAF
_
Pb (ug/L)
AA
_
STANDARD REFERENCE MATERIAL
1643C-1
1643C-1
Repl
Rep 2
certified
value
1641b
1641b
1641b
1641b
1641b
1641b
Rep 1
Rep 2
Rep 3
Rep 4
Rep 5
Rep 6
certified
value
REPLICATE ANALYSIS
379GLBR-
379GLBR-
379GLBR-
5 Rep 1
5 Rep 2
5 Rep 3
379GLBR- 121 Rep 1
379GLBR- 121 Rep 2
379GLBR- 121 Rep 3
07OCT12:381SAL
07OCT12:381SAL
07OCT12:381SAL
RSD%
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
RSD%
U = Detected at or below detection limit.
NA «= Not applicable/analyzed.
RSD % = Relative Standard Deviation
18.90
18.37
19.00
±0.6
MA
MA
MA
MA
NA
MA
NA
NA
27.9
30.1
22.3
±2.8
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
1372
1452
1484
1596
1572
1454
1520
±40
36.43
35.42
35.3
±0.9
NA
NA
NA
NA
NA
NA
NA
NA
0.40
0.36
0.36
6%
0.22
0.22
0.36
30%
13.6
11.2
11.7
10%
5.3
4.4
2.9
29%
0.00216
0.00094 U
0.00094 U
NA
0.00047 U
0.00047 U
0.00094 U
NA
21.95
19.88
17.39
12%
3.08
3.08
1.54
35%
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(SBLT SEDIMENT EXTRACTIONS)
MSLCode
379GLBR- 5
379GLBR- 5
379GLBR- 5
379GLBR- 8
379GLBR- 121
379GLBR- 121
379GLBR- 121
379GLBR- 154
379GLBR- 460
379GLBR- 461
379GLBR- 464
379GLBR- 465
Rep 1 Fraction
Fraction
Fraction
Fraction
Rep 2 Fraction
Fraction
Fraction
Fraction
Rep 3 Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Rep 1 Fraction
Fraction
Fraction
Fraction
Rep 2 Fraction
Fraction
Fraction
Fraction
Rep 3 Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
Fraction
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
1
1
Sponsor ID
I BIN A
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
070CT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:381 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
07OCT1 2:301 SAL
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
23OCT4:354SA2M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
25OCT9:104SA3M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:455SA2M
4DEC11:555SA2M
4DEC11:555SA2M
4DEC11:555SA2M
4DEC11.-555SA2M
4DEC11:305SA3M
4DEC11:375SA3M
Cr (ug/L) Cu (ug/L)
AA AA
0
0
0
0
0
0
0
1
0
0
0
0
0
0
0
.50
.50
.50
.75
.50
.38
.38
.26
.50
.76
.76
.50
.23 U
.23 U
.23 U
0.23 U
0.87
0.22
0.36
0.36
0.23 U
0.23 U
0.23
0.23 U
0.23 U
0.23 U
0.29
0
1.
0.
0.
0.
8.
6.
5.
9.
8.
6.
5.
7.
13.
11.
29
01
64
65
65
40
70
90
80
70
80
70
90
10
20
1.9 U
1.9 U
5.2
2.8
1.9 U
1.9 U
3.6
3.2
1.9 U
1.9 U
2.4
2.0
5.6
2.2
1.9 U
1.9 U
1.7
0.8
2.5
2.5
0.8
0.8
2.1
2.1
0.73 U
1.3
2.1
1.3
20.1
14.2
5.9
5.9
70.7
35.8
25.7
22.3
53.5
34.5
25.7
20.2
16.9
13.2
Hg (ug/L)
CVAF
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.00094
.00047
.00060
.00047
.00094
.00047
.00069
.00047
.00047
.00047
.00047
.00047
.00047
.00047
.00047
.00047
.00047
00024
0.00024
0.00024
0.00047
0.00024
0.00024
Pb (ug/L)
AA
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.00026
0.00024
0.00024
0.00024
U
U
U
0.00035
0.00149
0.00066
0
0
0
0.
0.
0.
0.
0.
0.
0.
0.
0.
00255
00197
00156
00024
00076
00091
00066
00036
00107
00054
00024
00036
U
0.72
0.72
6.63
4.56
1.66
0.83
5.80
3.31
1.24
1.66
4.56
2.07
1.18
1.18
1.18
1.18
0.60
0.60
1.00
1.33
0.60
0.67
1.00
1.67
0.60
0.60
2.00
1.33
0.72
0.72
3.82
4.77
7.23
6.37
2.31
0.87
8.39
6.65
4.05
0.87
6.91
6.50
U
U
U
U
U
U
U
U
U
U
U
U
U
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(SBLT SEDIMENT EXTRACTIONS)
MSLCode
379GLBR- 462
379GLBR- 463
379GLBR- 7
379GLBR- 1 0
379GLBR- 214
379GLBR- 250
379GLBR- 466
379GLBR- 467
379GLBR- 468
379GLBR- 469
379GLBR- 470
379GLBR- 471
Sponsor ID
-
I BIN A
Fraction 1 4DEC12:055SA2M
Fraction 2 4DEC12:055SA2M
Fraction 3 4DEC12:055SA2M
Fraction 4 4DEC12:055SA2M
Fraction 1 4DEC11:155SA3M
Fraction 2 4DEC11:155SA3M
Fraction 3 4DEC11:155SA3M
Fraction 4 4DEC11:155SA3M
I BIN B
Fraction 1 07OCT12:571SBL
Fraction 2 07OCT1 2:571 SBL
Fraction 3 07OCT1 2:571 SBL
Fraction 4 07OCT1 2:571 SBL
Fraction 1 07OCT1:071SBL
Fraction 2 07OCT1 :071 SBL
Fraction 3 07OCT1:071SBL
Fraction 4 07OCT1:071SBL
Fraction 1 31OCT9:304SB2M
Fraction 2 31OCT9:304SB2M
Fraction 3 31OCT9:304SB2M
Fraction 4 31OCT9:304SB2M
Fraction 1 31OCT2:404SB3M
Fraction 2 31OCT2:404SB3M
Fraction 3 31OCT2:404SB3M
Fraction 4 31OCT2:404SB3M
Fraction 1 4DEC12:505SB2M
Fraction 2 4DEC12:505SB2M
Fraction 3 4DEC12:505SB2M
Fraction 4 4DEC12:505SB2M
Fraction 1 4DEC1:005SB2M
Fraction 1 4DEC1:155SB2M
Fraction 1 4DEC1:255SB1/B3M
Fraction 2 4DEC1:255SB1/B3M
Fraction 3 4DEC1:255SB1/B3M
Fraction 4 4DEC1:255SB1/B3M
Fraction 1 4DEC1:305SB1/B3M
Fraction 1 4DEC1:355SB1/B3M
Cr (ug/L)
AA
I
8.00
7.00
8.20
9.20
9.50
8.80
12,50
13.60
I
0.23 U
0.30
0.38
0.23
1.40
1.30
1.70
1.00
0.23 U
0.23 U
0.23 U
0.23 U
0.60
0.50
0.70
0.70
15.40
15.30
14.60
14.80
10.00
9.90
3.68
3.22
3.95
4.96
6.90
7.70
Cu (ug/L)
AA
56.4
35.8
27.4
23.6
10.5
6.7
5.5
5.1
0.73 U
0.73 U
3.8
1.3
8.0
6.6
8.9
7.1
2.4
1.9 U
1.9 U
1.9 U
4.7
1.9
5.2
3.3
15.5
9.4
8.5
6.6
17.9
17.4
133.2
88.3
81.3
64.6
121.7
121.3
Hg (ug/L)
CVAF
0.00082
0.00040
0.00087
0.00098
0.00031
0.00030
0.00051
0.00045
0.00047 U
0.00047 U
0.00024 U
0.00039
0.00047
0.00024 U
0.00024 U
0.00025
0.00047 U
0.00047 U
0.00047 U
0.00055
0.00054
0.00064
0.00113
0.00143
0.00024 U
0.00024 U
0.00040
0.00030
0.00027
0.00027
0.00047 U
0.00047 U
0.00047 U
0.00047 U
0.00133
0.00132
Pb (ug/L)
AA
8.68
8.10
4.34
1.16
7.81
5.50
5.21
4.34
0.60 U
0.60 U
3.81
0.69
9.83
9.17
10.81
9.17
0.72 U
0.72 U
0.72 U
0.72 U
0.57 U
0.62
3.71
3.09
7.72
6.50
6.10
4.06
6.50
6.10
10.98
5.66
1.77
0.72 U
18.70
10.57
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(SBLT SEDIMENT EXTRACTIONS)
MSLCode
BLANK-1
BLANK-1
BLANK-1
BLANK-1
BLANK-2
BLANK-2
BLANK-2
BLANK-2
BLANK-3
BLANK-3
BLANK-3
BLANK-3
STANDARD
1643C-1
1643C-1
1643C-2
1643C-2
1643C-3
1643C-3
1643C-4
1641b
1641b
1641b
1641b
1641b
1641b
1641b
Sponsor ID
Fraction 1
Fraction 2 ;
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
Fraction 1
Fraction 2
Fraction 3
Fraction 4
REFERENCE MATERIAL
Rep1
Rep 2
Rep1
Rep 2
Rep1
Rep 2
Rep 1
certified
value
Rep 1
Rep 2
Rep 3
Rep 4
Rep 5
Rep 6
Rep 7
certified
value
Cr (ug/L) Cu
AA
0.23 U
0.23 U
0.23 U
0.23 U
0.30
0.23 U
0.30
0.23 U
0.20 U
0.50
0.20 U
0.20 U
19.59
20.81
19.50
19.10
19.80
19.40
NA
19.00
±0.6
NA
NA
NA
NA
NA
NA
NA
NA
NA
(ug/L)
AA
1.9 U
1.9 U
1.9 U
1.9U
0.73 U
0.73 U
0.80
0.73 U
0.90
0.82 U
0.82 U
0.82 U
27.5
25.8
26.5
26.5
26.3
25.9
NA
22.3
±2.8
NA
NA
NA
NA
NA
NA
NA
NA
NA
Hg (ug/L)
CVAF
0.00047
0.00047
0.00047 U
0.00047 U
0.00024 U
0.00024 U
0.00024 U
0.00032
0.00070
0.00028
0.00058
0.00026
NA
NA
NA
NA
NA
NA
NA
NA
NA
1465
1367
1442
1504
1440
1530
1518
1520
±40
Pb (ug/L)
AA
0.72 U
0.72 U
0.72 U
0.72 U
0.60 U
0.60 U
0.60 U
0.60 U
0.57 U
0.57 U
0.57 U
0.57 U
35.56
36.48
36.92
37.85
33.74
36.95
37.56
35.30
±0.90
NA
NA
NA
NA
NA
NA
NA
NA
NA
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
METALS IN LEACHATE SAMPLES
(SBLT SEDIMENT EXTRACTIONS)
MSLCode Sponsor ID
REPLICATE ANALYSIS
379GLBR- 5 Rep 1 Fraction 1 07OCT1 2:381 SAL
379GLBR- 5 Rep 2 Fraction 1 07OCT1 2:381 SAL
379GLBR- 5 Rep 3 Fraction 1 07OCT1 2:381 SAL
RSD%
379GLBR- 5 Rep 1 Fraction 2 07OCT1 2:381 SAL
379GLBR- 5 Rep 2 Fraction 2 07OCT1 2:381 SAL
379GLBR- 5 Rep 3 Fraction 2 07OCT1 2:381 SAL
RSO%
379GLBR- 5 Rep 1 Fraction 3 07OCT1 2:381 SAL
379GLBR- 5 Rep 2 Fraction 3 07OCT1 2:381 SAL
379GLBR- 5 Rep 3 Fraction 3 07OCT12:381SAL
RSD%
379GLBR- 5 Rep 1 Fraction 4 07OCT1 2:381 SAL
379GLBR- 5 Rep 2 Fraction 4 07OCT1 2:381 SAL
379GLBR- 5 Rep 3 Fraction 4 07OCT1 2:381 SAL
RSO%
379GLBR-121 Rep 1 Fraction 1 23OCT4:354SA2M
379GLBR- 121 Rep 2 Fraction 1 23OCT4:354SA2M
379GLBR-121 Rep 3 Fraction 1 23OCT4:354SA2M
RSO%
379GLBR- 121 Rep 1 Fraction 2 23OCT4:354SA2M
379GLBR-121 Rep 2 Fraction 2 23OCT4:354SA2M
379GLBR- 121 Rep 3 Fraction 2 23OCT4:354SA2M
RSO%
379GLBR-121 Rep 1 Fraction 3 23OCT4:354SA2M
379GLBR- 121 Rep 2 Fraction 3 23OCT4:354SA2M
379GLBR- 121 Rep 3 Fraction 3 23OCT4:354SA2M
RSD%
379GLBR-121 Rep 1 Fraction 4 23OCT4:354SA2M
379GLBR-121 Rep 2 Fraction 4 23OCT4:354SA2M
379GLBR-121 Rep 3 Fraction 4 23OCT4:354SA2M
RSO%
Cr (ug/L) Cu
AA
0.50
0.50
0.50
0%
0.50
0.38
0.76
35%
0.50
0.38
0.76
35%
0.75
1.26
0.50
46%
0.87
0.22
0.36
71%
0.36
0.23 U
0.23 U
NA
0.23
0.23 U
0.23 U
NA
0.36
0.23 U
0.29
22%
(ug/L)
AA
1.9 U
1.9 U
1.9 U
NA
1.9 U
1.9 U
1.9 U
NA
5.2
3.6
2.4
38%
2.8
3.2
2.0
23%
1.7
0.8
0.73 U
72%
0.8
0.8
1.3
30%
2.5
2.1
2.1
10%
2.5
2.1
1.3
33%
Hg (ug/L)
CVAF
0.00094 U
0.00094 U
0.00047 U
NA
0.00047 U
0.00047 U
0.00047 U
NA
0.00060
0.00069
0.00047 U
14%
0.00047 U
0.00047 U
0.00047 U
NA
0.00047 U
0.00047 U
0.00024 U
NA
0.00024 U
0.00024 U
0.00024 U
NA
0.00024 U
0.00024 U
0.00024 U
NA
0.00024 U
0.00026
0.00035
30%
Pb (ug/L)
AA
0.72 U
1.66
1.24
29%
0.72 U
0.83
1.66
67%
6.63
5.80
4.56
18%
4.56
3.31
2.07
38%
0.60 U
0.60 U
0.60 U
NA
0.60 U
0.67
0.60 U
NA
1.00
1.00
2.00
43%
1.33
1.67
1.33
16%
U - Detected at or below detection limit.
NA * Not applicable/analyzed.
NS = Not spiked.
RSD % « Relative Standard Deviation.
Page 4
-------
REPORT OF CHEMICAL ANALYSES
Volume 3: Organics
PROJECT: Buffalo River Pilot Project
Prepared for:
USEPA Great Lakes National Program Office
Attn: Mr. Steve Garbaciak
230 S. Dearborn
Chicago, IL 60604
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: BUFFALO RIVER PILOT PROJECT DATE: May 26, 1992
ISSUEDTO: Mr. Steve Garbaciak CF#: 379GLBR
Technical Project Manager
USEPA Great Lakes National Program Office
230 S. Dearborn
Chicago, IL 60604
INTRODUCTION
This report summarizes the results from analyses performed on pilot study samples which were
submitted by the U.S. Army Corps of Engineers Great Lakes Division, Buffalo District.
SAMPLE CUSTODY
Samples were received in good condition from October 7, 1991 through December 5, 1991. Samples
were logged in and stored as specified in the narrative. Samples were analyzed within the holding times
specified in the QA plan. Any exceptions are noted in the narrative associated with each analysis.
AIR SAMPLES
Five samples and one solvent blank were analyzed for dioxin/furans, PAH's and PCB's. Samples were
stored at 4°±2°C prior to shipment to Twin City Testing for analysis of dioxin/furans, PAHs and PCBs.
The samples were extracted in their entirety, therefore re-analysis was not possible. Included with
this report are copies of the text which accompanied Twin City Testing's report for the air samples.
Please refer to that data for information on extraction, analysis, quality control and any problems
associated with analysis of the air samples. No samples were received to be archived.
SAMPLE IDENTIFICATION
Sponsor ID Sample Type Analyses Battelle ID
22OCT5:0011GA1O Air D/F, PAH, PCB 379GLBRM12
23OCT4:4511GA2O Air D/F, PAH, PCB 379GLBR*232
24OCT53011GA3O Air D/F, PAH, PCB 379GLBR*233
25OCT1:4511GB1O Air . D/F, PAH, PCB 379GLBR*234
31OCT1:0011GB3O Air D/F, PAH, PCB 379GLBR*272
SEDIMENT and WATER SAMPLES
Fifty-one sediment samples were analyzed for PAHs and oil and grease. Forty-six sediment samples
were analyzed for PAHs, PCBs and oil and grease. Samples were stored at -22°±3°C prior to analysis.
Oil and grease in sediment was determined according to "SOP for the Analysis of Solvent-Extractable
Residue from Whole Sediment" taken from EPA-LLRS-GROSSE and supplied by the Great Lakes Large
Lakes Lab. Twenty-three water samples were analyzed for PAHs, PCBs and oil and grease. Samples
were stored at 4°±2°C prior to analysis. Since the organics lab extracted the entire sample for PAH
and PCB analysis, and oil and grease used most of the duplicate sample, re-extractions were virtually
impossible. On one occasion the organic samples were logged in incorrectly, as though each sample
(including the duplicates) was a separate sample with each receiving an individual sample ID. In these
-------
instances, the organics analyst extracted each sample in it's entirety, leaving no sample for oil and
grease. To compensate for this error, metals samples or TOC samples collected from the same time and
point of the processor were extracted for oil and grease. Although the metals and TOC samples had been
preserved with acid, according to Standard Methods, acidifying an oil and grease sample does not affect
the results. Oil and grease in water was determined following Standard Methods, 5520B, substituting
methylene chloride for freon. Most water samples posed a problem using this method due to a high
content of paniculate matter in the sample. After some discussion with Eric Crecelius (program
manager), the analyst was instructed to decant and extract the liquid layer. The paniculate fraction
was not extracted, but was archived for possible analysis in the future.
Water samples for PAHs and PCBs were extracted by shaking with methylene chloride in a targe
separatory funnel. Three consecutive extractions were performed on each sample, exchanginq solvent
after each extraction period following SOP IMSL-M-41. Samples were then cleaned using
Silica/Alumina (5% deactivated) chromatography, followed by HPLC cleanup (Krahn et al. 1988).
PAH extracts were analyzed using Gas Chromatography/Mass Spectrometry (GC/MS) in the selected ion
mode (SIM). PCB extracts were analyzed using Gas Chromatography/Electron Capture Detection
(GC/ECD). The column used was a J&W DB-5 capillary column (30m x 0.25mm I.D.). Sediment
samples for PAHs and PCBs were extracted with methylene chloride using the ambient rolling
technique. Three consecutive extractions were performed on each sample, exchanging solvent after
each extraction period following SOP fMSL-M-42. Samples were then cleaned using Silica/Alumina
(5% deactivated) chromatography followed by HPLC cleanup (Krahn et al. 1988). Extracts for PAHs
were analyzed using Gas Chromatography/Mass Spectrometry (GC/MS) in the selected ion mode (SIM).
Extracts for PCBs were analyzed using Gas Chromatography/Electron Capture Detection (GC/ECD). The
column used was a J&W DB-5 capillary column (30m x 0.25mm I.D.).
For the majority of water samples to be analyzed for PAHs and PCBs, extraction exceeded the
recommended 7-day holding time. However, due to the stable nature of PCB compounds and storage
methods, the quality of the data should not be affected. Holding times from extraction to initial analyses
were generally within EPA's recommended holding time of 40 days (EPA 1986). However, diluted
samples were run approximately 30 to 40 days outside of these holding times. Values for diluted
sample analyses generally agreed well with the initial quantitation, therefore, this added time does not
appear to have biased the diluted results. Sediment samples for PAHs were extracted in 5 batches from
2/6/92 to 3/4/92 and analyzed from 3/31/92 to 4/18/92. Samples that required re-analysis were
extracted on 4/22/92 and analyzed on 5/4/92. Samples that required dilution were analyzed on
5/1/92. One batch of sediment analyses requested as a rush by EPA GLNPO were extracted on
10/10/91 and analyzed on 10/14/92. Sediment samples for PCBs were extracted simultaneously
with those for PAHs and analyzed from 4/20/92 through 4/26/92.
Target detection limits of 0.02 u,g/L for PAHs in water were slightly exceeded in a number of cases.
Detection limits ranged from 0.007 jig/L to 0.07 pg/L. In general, levels of PAHs exceeded these
amounts in all but three samples. Target detection limits of 0.01 u.g/L for PCBs in water were slightly
exceeded for Aroclors. Detection limits averaged 0.05 u.g/L to 0.2 u,g/L for undiluted samples and from
0.5 to 2 u-g/L for diluted samples. In most cases, PCBs in the samples analyzed exceeded these amounts.
Sediment PAH target detection limits of 0.02 ng/Kg were slightly exceeded, ranging from 0.004 to
0.053 jig/Kg. Sediment PCB target detection limits of 0.02 u,g/Kg were slightly exceeded, ranging
from 0.025 to 0.060 u,g/Kg. Detection limits reported were instrument detection limits based on a
minimum area, background noise and the analyst's judgement on the level that was quantifiable.
-------
SAMPLE IDENTIFICATION
Sponsor ID
07OCT12:341 SAO
07OCT1:101SBO
07OCT12:401 SAO
07OCT1331SCO
07OCT2:041SDO
07OCT1:441SCO
07OCT1.-011SBO
07OCT2:121SDO
08OCT5:402SD1O
08OCT5302SD2O
09OCT11:502SA3O
09OCT11:282SA1O
09OCT10:152SB2O
09OCT10:352SB3O
09OCT4:352SC2O
09OCT4:162SC3O
22OCT5:563SA20
23OCT1:303SA2O
23OCT4284SA2O
23OCT4294SA2O
24OCT2203SA3O
24OCT5:503SA3O
25OCT9224SA3O
25OCT9:224SA3O
250CT2:153SB1O
250CT2:294SB1O
25OCT2:284SB1O
30OCT2:493SB2O
30OCT4:413SB2O
31OCT9:264SB2O
31OCT9:254SB20
31OCT10:453SB30
31OCT2:303SB3O
31OCT2:384SB3O
31OCT2:364SB3O
18NOV2:553SC1O
18NOV4:403SC1O
19NOV9:004SC1O
19NOV9:014SC1O
19NOV2:203SC2O
19NOV3:553SC20
19NOV4:504SC2O
19NOV4:504SC2O
20NOV1:003SC3O
20NOV1:553SC3O
20NOV3:154SC3O
20NOV3:154SC3O
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment -
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH. Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
Battelle ID
379GLBR*13
379GLBFT14
379GLBRM6
379GLBR*18
379GLBR*19
379GLBR*20
379GLBR*23
379GLBR*24
379GLBR*51
379GLBR*53
379GLBR*57
379GLBR*59
379GLBR*66
379GLBR*67
379GLBR*74
379GLBR*75
379GLBR*111
379GLBR*113
379GLBR*122
379GLBR*124
379GLBR*141
379GLBRM43
379GLBRM51
379GLBRM52
379GLBR*176
379GLBRM82
379GLBRM83
379GLBRM98
379GLBR*206
379GLBR*220
379GLBR*221
379GLBR*242
379GLBR*244
379GLBR*247
379GLBR*249
379GLBR*280
379GLBR*284
379GLBR*303
379GLBR*304
379GLBR*313
379GLBR*315
379GLBR*324
379GLBR"325
379GLBR*342
379GLBR*344
379GLBR*351
379GLBR*352
-------
21NOV12.-003SD1O
21NOV2:433SD1O
21NOV5:224SD1O
21NOV5:224SD1O
07OCT1211SCO
07OCT12:091 SAO
07OCT12:531 SBO
07OCT1S21SDO
08OCT5:132SD3O
09OCT11:382SA2O
09OCT9:542SB1O
09OCT4362SC1O
22OCT11:317SA1O
22OCT11:378SA1O
22OCT4203SA2O
23OCT4:274SA2O
24OCT10:457SA2O
240CT10:508SA2O
24OCT6:203SA3O
25OCT9:214SA3O
25OCT9:307SA3O
25OCT9:368SA3O
25OCT12:153SB1O
250CT2:254SB1O
25OCT3:527SB1O
25OCT3:578SB1O
30OCT2:573SB2O
31OCT9:027SB2O
31OCT9:078SB2O
31OCT9:244SB2O
31OCT11:503SB3O
31OCT2:354SB3O
1NOV10:208SB3O
1NOV10:157SB3O
18NOV3:503SC1O
19NOV9:347SC1O
19NOV8:594SC1O
19NOV9:238SC1O
19NOV11:303SC2O
19NOV4:504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV3.-154SC30
20NOV3.-337SC3O
20NOV3:278SC3O
21NOV1:353SD1O
21NOV5:078SD10
21NOV5:107SD1O
21NOV5:224SD1O
230CT4:459LA2O
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Oil
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH,
PAH.
PAH,
PAH,
PAH,
Oil&
Oil&
Oil&
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
PCB,
Gr
Gr
Gr
Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
Oil & Gr
379GLBFT376
379GLBFT380
379GLBFT396
379GLBFT397
379GLBRM5
379GLBFT17
379GLBFT21
379GLBFT22
379GLBRM6
379GLBFT58
379GLBR*65
379GLBR"73
379GLBR*104
379GLBRM07
379GLBR*108
379GLBRM23
379GLBRM36
379GLBRM39
379GLBR*145
379GLBRM53
379GLBRM66
379GLBRM67
379GLBRM74
379GLBRM81
379GLBRM93
379GLBRM96
379GLBRM99
379GLBR*210
379GLBR*213
379GLBR*222
379GLBR*243
379GLBR*248
379GLBR*268
379GLBR*269
379GLBR*282
379GLBR*288
379GLBR*302
379GLBR*307
379GLBR*311
379GLBR*323
379GLBR*337
379GLBR*340
379GLBR*350
379GLBR*357
379GLBR*360
379GLBR*378
379GLBR*384
379GLBR*388
379GLBR*395
379GLBR*128
-------
23OCT5:2010LA2O Water
25OCT10:1810LA3O Water
25OCT10:1910LA3O Water
25OCT10:201 OLA3M Water
25OCT9:549LA3O Oil
250CT10:009LA3C Oil
25OCT3:0810LB1O Water
30OCT4:206LA3O Water
31OCT10:119LB2O Oil
31OCT10:231 OLB20 Water
31OCT3:119LB3O Oil
31OCT3:109LB3O Oil
31OCT2:5710LB3M Water
31OCT3:069LB3M Oil
31OCT3:0110LB3O Water
31OCT3:0010LB3O Water
6NOV12:003LO Water
18NOV5:559LC1O Oil
18NOV6:1510LC1O Water
19NOV5519LC2O Oil
19NOV5:0510LC2O Water
20NOV2:193LC3O Water
20NOV2:419LC3O Oil
20NOV3:0110LC3O Water
21NOV3-.2610LD10 Water
21NOV4:169LD1O Oil
PAH, PCB, Oil & Gr
PAH, PCB
PAH, PCB
Oil & Gr (metals)
PAH, PCB
Oil & Gr (TOC)
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB
PAH, PCB
Oil & Gr (metals)
Oil & Gr (metals)
PAH, PCB
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
'Samples extracted for PAH and PCB only.
"Samples extracted for oil/grease and metals or TOC.
VSample was not analyzed.
ARCHIVED SAMPLES
Sponsor ID
21OCT12:483SA1O
21OCT12:493SA1O
21OCT5:444SA1O
21OCT5:464SA1O
22NOV12:153SD2O
22NOV1:153SD2O
22NOV3:104SD2O
22NOV3:104SD2O
25NOV1:003SD3O
25NOV1:403SD3O
25NOV4:004SD3O
25NOV4.-004SD3O
08OCT5:102SD3O
08OCT5:112SD3O
08OCT5:122SD3O
08OCT5:132SD3O
21OCT12:473SA1O
Sample Type
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Sediment
Analyses
PAH, Oil&Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil&Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PAH, Oil & Gr
PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
379GLBRM32
379GLBRM60*
379GLBR*161*
379GLBRM63**
379GLBRM64*
379GLBRM65**
379GLBR*187
379GLBR*204
379GLBR*226
379GLBR*227
379GLBR*252*
379GLBR*253'
379GLBR*254"
379GLBR*255"
379GLBR*256*
379GLBR*257
379GLBR*275
379GLBR*286
379GLBR*287¥
379GLBR*326
379GLBR*331
379GLBR*361
379GLBR*366
379GLBR*370
379GLBR*398
379GLBRM04
Battelle ID
379GLBR*83
379GLBR*84
379GLBR*92
379GLBR*93
379GLBRM08
379GLBRM09
379GLBRM18
379GLBRM19
379GLBR*436
379GLBRM38
379GLBRM44
379GLBRM50
379GLBRM6-T1
379GLBRM6-T2
379GLBRM6-T3
379GLBRM6-M1
379GLBR*82
-------
21OCT5:454SA1O Sediment
30OCT2:473SB2O Sediment
30OCT4:013SB2O Sediment
30OCT2:523SB2O Sediment
30OCT4:453SB20 Sediment
19NOV4:504SC2O Sediment
19NOV4:504SC2O Sediment
19NOV4:504SC2O Sediment
19NOV4:504SC20 Sediment
20NOV2:193LC30 Sediment
21NOV5:078SD1O Sediment
21NOV5:078SD1O Sediment
21NOV5:078SD1O Sediment
21NOV5:078SD10 Sediment
22NOV1:453SD2O Sediment
22NOV3:104SD2O Sediment
22NOV3:308SD20 Sediment
25NOV2:203SD3O Sediment
25NOV4-.004SD3O Sediment
21OCT6:1810LA1O Water
21OCT6:2010LA1O Water
21OCT6:2210LA1O Water
21OCT6:1610LA1O Water
23OCT4:459LA2O Water
23OCT4-.459LA2O Water
23OCT4:459LA2O Water
230CT5:2010LA2O Water
23OCT5:2010LA2O Water
23OCT5:2010LA20 Water
25OCT3:0710LB1O Water
30OCT4:206LA3O Water
31OCT10:129LB2O Oil
31OCT10:2110LB2O Water
6NOV12:003LO Water
18NOV5:559LC1O Oil
18NOV5:559LC1O Oil
18NOV5:559LC1O Oil
18NOV5:559LC1O Oil
18NOV5:559LC1O Oil
18NOV6:1510LC1O Water
19NOV5:519LC2O Oil
19NOV5:0510LC2O Water
19NOV5:0510LC2O Water
19NOV5:0510LC2O Water
19NOV5:0510LC2O Water
20NOV2:419LC3O Oil
20NOV3:0110LC3O Water
21NOV3:2610LD1O Water
21NOV4:169LD1O Oil
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
379GLBR*91
379GLBR*199-T1
379GLBR*199-T2
379GLBRM99-M1
379GLBR*199-M2
379GLBR'323-T1
379GLBR*323-T2
379GLBR*323-M1
379GLBR*323-M2
379GLBR*361-1
379GLBR*384-T1
379GLBR*384-T2
379GLBR*384-M1
379GLBR*384-M2
379GLBR*412
379GLBRM17
379GLBRM23
379GLBRM40
379GLBRM49
379GLBR*97
379GLBR*97-T1
379GLBR*97-T2
379GLBR*97-T3
379GLBR*128-1
379GLBR*128-2
379GLBR*128-3
379GLBR*132-1
379GLBRM32-2
379GLBRM32-3
379GLBR*187-1
379GLBR*204-1
379GLBR*226-1
379GLBR*227-1
379GLBR*275-1
379GLBR*286-1
379GLBR*286-T1
379GLBR'286-T2
379GLBR"286-M1
379GLBR*286-M2
379GLBR*287-1
379GLBR*326-1
379GLBR*331-T1
379GLBR*331-T2
379GLBR*331-M1
379GLBR*331-M2
379GLBR*366-1
379GLBR*370-1
379GLBR*398-1
379GLBRM04-1
-------
21NOV4:169LD1O
21NOV4:169LD1O
21NOV4:169LD1O
21NOV4:169LD1O
22NOV2:3010LD2O
22NOV2:3010LD2O
22NOV2:539LD2O
22NOV2:539LD20
25NOV4:0010LD3O
25NOV4:0010LD3O
25NOV4:009LD3O
25NOV4:009LD3O
Oil
Oil
Oil
Oil
Water
Water
Oil
Oil
Water
Water;
Oil
Oil
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
PAH, PCB, Oil & Gr
379GLBFT404-T1
379GLBRM04-T2
379GLBRM04-M1
379GLBRM04-M2
379GLBRM26
379GLBRM26-1
379GLBRM31
379GLBRM31-1
379GLBRM52
379GLBRM52-1
379GLBRM53
379GLBRM53-1
OIL AND GREASE
Analysis of oil and grease in water following the SOP which we received from the Large Lakes Lab was
not possible. Most of the samples had a very high content of oil and fine sediment. When the sample was
shaken, only one phase was apparent instead of two as described in the method. Consequently, after
discussion with Eric Crecelius (program manager), the analyst allowed the sediment to settle, decanted
and analyzed the liquid, and archived the sediment. Some sediment samples analyzed for oil and grease
were rerun due to the formation of a drying agent residue in the extract which caused higher values. In
some cases, ash passed through the filter into the extract, which caused higher values. In other cases,
the replication between field replicates was not in good agreement. We wanted to ensure that the poor
agreement was due to some artifact other than the methodology. If the reruns differed substantially
from the original value obtained, the rerun value was reported. If the differences were slight, the
original value was reported. All samples were analyzed outside the standard EPA holding time of 28
days. This was due in part to the addition of this analysis to the sampling scheme after the program was
underway and partially to sample backlog in the organics laboratory. The quality of the data should not
be affected since the sediments were stored at -22°±5°C and the water samples were stored at 4°±2°C
prior to analysis. Matrix spikes for sediments were within the criteria outlined in the QAPP for
organic samples, except for samples 379GLBR*182 and 384 which were treated sediment. Recoveries
were higher in those samples probably due to matrix interference.
PAHS AND PCBS
Water
Matrix problems were evident in these samples due to high concentrations of oil. Many spike and
surrogate recoveries were outside of the criteria. EPA GLNPO (Rick Fox) indicated they wanted the
entire sample extracted, including the oil adhered to the sides of the bottles. When the analysts
extracted the samples, they found that the methylene chloride formed an emulsion with the oily water
which could not be separated out. This caused a problem in the clean-up step and apparently caused
some matrix interference in the samples. Evidence for this assumption comes from spike blank
recoveries, replicate RSDs and blank data, which were within the established ARCS criteria.
One method blank was extracted and analyzed for PAHs with the samples. Naphthalene and
Benzo(ghi)perylene were detected at levels near detection limits in the blank. These levels were less
than five times the levels found in all but three samples. The corresponding sample values for these
samples were flagged with a "B" to indicate a possible bias due to blank contamination. One method
-------
blank was extracted and analyzed for PCB Aroclors with the samples. No PCBs were detected in the
method blanks.
Three stable isotopically labelled PAH compounds were added as surrogates prior to extraction to assess
the efficiency of the analysis. The majority of recoveries for all three surrogates were generally below
the lower QC limits (40-120%). This is mainly due to very high PAH concentrations and oily material
associated with these samples. Performing an efficient extraction on these samples was very difficult.
Samples with little or no PAHs had much higher surrogate recoveries, including the method blank. Due
to limited sample volumes, holding times and extremely difficult sample matrices, no re-extractions
were performed. Overall, PAH levels may be somewhat biased low based on the surrogate recoveries.
However, the values for some of the higher weight PAH compounds are nearing their solubility limit in
water and the levels quantified are more likely a function of the amount of oily material in the sample
rather than a truly dissolved quantity. Two compounds, tetrachlorometaxylene (TCMX) and
octachloronaphthalene (OCN) were added as surrogates to all samples prior to extraction of PCBs to
assess the efficiency of the analysis. Recoveries of four samples for TCMX and OCN slightly exceeded the
QC guidelines of 40-120%. All recoveries were above 20%, therefore no re-extractions were
performed.
One sample was spiked in duplicate with a PAH standard (see MSL-M-42). However, the level spiked
was generally five to ten times tower than the amount in the native sample. This precluded accurate
determination of spike recoveries for all but one compound, benzo(k)fluoranthene, which was not
present above detection limits in the native sample. Recoveries for PAHs were generally poor due to
matrix interference and non-homogenous samples. In addition, spike concentrations were generally
lower than the sample concentration, therefore were difficult to detect. For PCBs, one sample was
spiked in duplicate with Aroclor 1254. Unfortunately, it appears that one of the two samples was not
spiked after all, therefore matrix spike recoveries were only reported for one of the two samples.
Aroclor 1254 spike recovery was 112% for this sample.
One sample was extracted in triplicate to assess the precision of PAH analyses. RSD values ranged from
4 to 40%. The majority of RSD values were between 20-30%, which exceeds the precision goal of
20%. These values indicate relatively good precision, considering high levels of PAHs in the samples
and the difficulty of performing representative extractions on these oily, complex matrices. One
sample was extracted in triplicate to assess the precision of PCB analyses. The sample analyzed
contained high levels of Aroclor 1248 and needed dilution prior to quantification. The RSD value for the
triplicate analyses was 41%. This exceeded the QAPP precision goal of 20%. Some error was
introduced due to dilution which contributed to the higher RSD value. In addition, these water samples
contained high levels of PCBs and oily material which are difficult to extract entirely from the samples.
Some variability may come from non-homogenous field replicates. The combination of these factors
most likely contributed to high RSD values.
Standard reference materials (SRMs) are not available for organics in water samples.
Sediments
Matrix problems were evident in these samples due to high concentrations of oil. Many spike and
surrogate recoveries were outside of the criteria. When the analysts extracted the samples, they found
that the methylene chloride formed an emulsion with the oily water content of the sediments which
could not be separated out. This caused a problem in the clean-up step and apparently caused some
matrix interference in the samples. Evidence for this assumption comes from spike blank recoveries,
replicate RSDs and blank data, which were within the established ARCS criteria.
8
-------
Seven method blanks, one with each batch, were extracted and analyzed for PAHs. Naphthalene and
Phenanthrene were detected at levels near detection limits. Sample concentrations were five times
these levels In all samples but three. One method blank was extracted with each batch for PCBs. No
PCBs were detected in the blanks.
our stable isotopically labelled PAH compounds were added as surrogates prior to extraction to assess
the efficiency of the analyses. Recoveriesof two of the surrogates d8 naphthalene and d10
acenaphthalene were occasionally low (<40%) due to their volatile nature. The surrogate d14 Dibenzo
(a.h) Anthracene was detected both above and below the acceptable limit. The tower values indicate that
this particular surrogate may be susceptible to degradation. We are presently replacing dl4 dibenzo
(a.h) anthracene with d10 pyrene in an effort to achieve better recoveries. Two compounds,
tetrachtorometaxylene (TCMX) and octachloronaphthalene (OCN) were added to all samples prior to
extraction for PCBs to assess the efficiency of the analyses. Recoveries for TCMX were within the QC
guidelines of 40-120%, except for one sample. OCN recoveries were generally high due to
underspiking, which caused difficulty in quantification of this surrogate.
Five samples and three blanks were spiked in duplicate with a PAH combined stock standard. Most
samples contained much higher concentrations of PAHs than were spiked, therefore spike recoveries
were usually outside the required criteria (40-120%). Matrix spikes with poor recoveries in which
the spike concentration was approximately the same as the sample or higher, are probably a result of
matrix interference. Matrix spikes for sample 379GLBR*46 were not reported because the sample
results were suspect from the first analysis, the sample was rerun producing very different results,
but the spikes were not rerun. Spike data for the initial analysis of sample 379GLBR*111 were not
reported as the results were questionable and the sample and spikes were re-analyzed. The reruns
were reported. Two samples and two method blanks were spiked in duplicate with Aroclor 1254 for
PCBs. Several recoveries were slightly above the acceptable limit (40-120%). One of the blank
spike recoveries was abnormally high, possibly due to an accidental duplicate spike on that sample.
Five samples were extracted in triplicate for PAHs to assess the precision of the analyses. Precision
was measured by calculating the relative standard deviation (RSD) between the replicate results for
each of 17 compounds. RSD values ranged from 3 to 25% for with one RSD of 52%. The majority of
the RSD values were between 10 and 20%, indicating good precision. Two samples were extracted in
triplicate for PCBs to assess the precision of the analyses. Sample 379GLBR*199 did not replicate
well with an RSD of 89% for the Aroclors detected, possibly due to uneven oil distribution within the
sediment matrix.
The SRM generally used for sediments (NIST 1941) is not certified for PCB Aroclors or PAHs, only
individual congeners. One other SRM is available and is certified for PCB Aroclor 1254, (HS-2 from
NRCC), however, it was originally certified using a packed column. Our experience has shown that
there is little or no 1254 pattern when capillary column GC is used. Therefore, we do not use it as a
SRM for Aroclors. SRM data is reported for PAHs and compared using RSD values.
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polynuclear Aromatic Hydrocarbons (PAHs)
Twin City Testing, Inc.
Air
SAMPLE NUMBER: 6
Reference Range of
Method Recovery
8270 40-120%
HOLDING TIMES Not specified.
Relative
Precision
±20%
Detection
Limit
N/A
DETECTION LIMITS Detection limits were different for each sample and each compound. Detection
limits ranged from 0.75 to 3.8 ng/sample. Please refer to the summary table for
specific detection limits.
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
SURROGATES
A laboratory method blank was prepared and analyzed with each sample
extraction batch. The blanks were free of the target PAH analytes, with the
exception of a trace background level (77 nanograms) of naphthalene. The
naphthalene levels determined for the affected samples were all higher than
the naphthalene level in the blank by 20 times or more. This indicates that the
sample processing steps did not contribute significantly to the levels reported
for the samples.
The amount of material was insufficient to prepare matrix spikes. Two
laboratory spike samples were prepared with the air sample batch. Spike
recoveries ranged from 52-132%, which are all within the 50-135% target
ranges designated for these analyses.
The amount of material was insufficient for the preparation of replicates.
SRMs are not available for PAHs in air samples.
The designated range for the surrogate compounds in the PAH samples is 50-
150% for at least two of the three surrogates in each sample. All the surrogate
recoveries in the PAH samples fell within this range, with the exception of
perdeuterated pyrene (227%) in sample 379GLBR*112ABE. Since the
remaining two surrogates in this sample were recovered at acceptable levels,
the recovery criteria were met and no corrective action was required. The raw
area count for the perdeuterated naphthalene internal standard in sample
379GLBR*272ABD was 269% of the value for the corresponding standard in
the daily continuing calibration analysis. THe target range for internal standard
areas in the sample extracts is 50-200% of the daily continuing calibration
values. Upon dilution of this sample extract, the naphthalene internal standard
area fell into the acceptable range.
10
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polychlorinated biphenyls (PCBs)
Twin City Testing, Inc.
Air
SAMPLE NUMBER: 6
Reference
Method
680
Range of
Recovery
40-120%
Relative
Precision
±20%
Detection
Limit
N/A
HOLDING TIMES Not specified.
DETECTION LIMITS Detection limits were different for each sample and each compound. Detection
limits ranged from 60 to 120 ng/sample. Please refer to the summary table for
specific detection limits.
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
SURROGATES
A laboratory method blank was prepared and analyzed with each sample
extraction batch. The blanks were free of the target PCB analytes. A low
recovery was achieved for the 2-Fluorobiphenyl surrogate in the PCB blank due
to inadvertent volatilization of this compound during the concentration steps.
Since the entire sample was consumed in the extraction process, any
reprocessing was not possible. The blank associated with the impinger
samples exhibited a low recovery (35%) for the perdeuterated anthracene
surrogate. Since good recoveries were achieved for the other two surrogates in
this blank, no corrective action was required.
The amount of material was insufficient to prepare matrix spikes. Two
laboratory spike samples were prepared with each batch. Spiked native
compounds were recovered at levels ranging from 52-132%, which are all
within the 50-135% target ranges designated for these analytes.
The amount of material was insufficient for preparation of replicates.
SRMs are not available for PCBs in air samples.
The recoveries of the surrogate compounds fell within the 50-125% guidelines
specified in Method 680, with the exception of the 2-Fluorobiphenyl recovery
(47%) in sample 379GLBRM12F.
1 1
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Dioxins/furans
Twin City Testing, Inc.
Air
SAMPLE NUMBER: 6
Reference
Method ;
EPA Method 23
HOLDING TIMES Not specified.
Range of
Recovery
Not specified
Relative
Precision
Not specified
Detection
Limit
Not specified
DETECTION LIMITS Detection limits were different for each sample and each compound. Generally,
they varied from 0.013 to 0.140 ng/sample. Please refer to the summary table
for specific detection limits.
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
SURROGATES
One laboratory method blank was prepared and analyzed with the sample
extraction batch. The blanks were free of dioxins and furans, with the exception
of trace background levels of PeCDD (19 picograms), HpCDD (6.3 picograms)
and OCDD (92 picograms). The levels determined for the affected isomers in
the actual samples were higher than the corresponding blank levels by 3-100
times. It should be noted, however, that levels less than five times higher than
the background are not generally considered statistically different from the
background.
The amount of sample material was insufficient to prepare matrix spikes. Two
quality control dioxin/furan spike samples were prepared with the sample batch.
The data show that the spiked native compounds were recovered at levels
ranging typically from 87-130%. The only compound with recoveries outside of
this range was 1,2,3,4,7,8,9-HpCDF, which exhibited a recovery of 160% in
each of the spike samples. It should be noted, that quality control ranges for
native spike sample recoveries are not specified in the method.
The amount of sample material was insufficient for the preparation of replicates.
SRMS are not available for dioxin/furans in air samples.
The recoveries of the isotopically-labeled dioxin/furan internal and surrogate
standards generally ranged from 70-130%. All the recoveries were within the
target ranges specified in the method, with the exceptions of the labeled
1,2,3,7,8-PeCDD in samples 379GLBRM12F (37%). 379GLBR*272ABD (37%),
and the lab spike duplicate (36%). Slightly elevated recoveries were obtained
for selected surrogate compounds in samples 379GLBR*233ABD (labeled
1,2,3,4,7,8-HxCDD, 145%), 379GLBR*272ABD (labeled 1.2,3,4,7,8-HxCDD,
148%), the laboratory spike (labeled 1,2,3,4,7,8,9-HpCDF, 135%). and the
laboratory spike duplicate (labeled 1,2,3,4,7,8,9-HpCDF, 135%). The native
1,2,3,7,8-PeCDD concentrations should be accurate for these samples since
12
-------
quantitation is based on isotope dilution. The native 1.2,3.4,7,8-HxCDD and
1,2,3,4,7,8.9-HpCDF concentrations in these four samples may, however, be
slightly elevated since both the native and surrogate isomers are compared to a
separate labeled isomer.
1 3
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
SAMPLE NUMBER:
Buffalo River Pilot Project
Oil and grease
Battelle Marine Science Laboratories
Water
23
Reference
Method
Range of
Recovery
Relative
Precision
±20%
Detection
Limit
HOLDING TIMES
DETECTION LIMITS
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
5520B 70-130% ±20% Not specified
Not specified.
The detection limit for this method was determined to be 1.1 mg/L.
Eight method blanks were prepared and analyzed, at least one with each batch
extracted. Oil and grease was less than the detection limit in all blanks.
Not required by the QAPP. Two samples were spiked in duplicate with a known
concentration of pump oil. Recoveries ranged from 95 to 134%. Laboratory
spike blanks (not required) were prepared and analyzed with recoveries
ranging from 76 to 78%.
Two samples were extracted and analyzed in triplicate. Relative standard
deviations were 3 and 17%.
SRMs are not available for oil and grease.
14
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Oil and grease
Battelle Marine Science Laboratories
Sediment
SAMPLE NUMBER: 97
Reference Range of
Method ; Recovery
EPA-LLRS-GROSSE 70-130%
HOLDING TIME Not specified.
Relative
Precision
+20%
Detection
Limit
N/A
DETECTION LIMIT The detection limit was determined as 630 p.g/g.
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
Nine blanks were prepared and analyzed; at least one with each batch. Oil and
grease was not detected in any of the blanks.
Not required in the QAPP. Five matrix spikes in duplicate were spiked with
pump oil, one with each batch. All recoveries were within 70-130%, with the
exception of 379GLBR*182 and 379GLBR*384, where recoveries ranged from
142 to 158%. These two samples were ash material which possibly caused
some matrix interference in this method. Laboratory blank spikes were
prepared and analyzed, with recoveries ranging from 87 to 115%.
Five samples were extracted and analyzed in triplicate; at least one per batch.
All triplicates were within the range of precision, with the exception of
379GLBRM11 and 379GLBR*384. Both samples replicated with a RSD of
22%, possibly caused by a residue from dissolution of sodium sulfate (drying
agent) when mixed with the sediment that passed through the filtration step into
the extract.
SRMs are not available for oil and grease.
15
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polynuclear Aromatic Hydrocarbons (PAHs)
Battelle Marine Science Laboratories
Water
SAMPLE NUMBER: 23
Reference
Method
MSL-M-41
Range of
Recovery
40-120%
Relative
Precision
+20%
Detection
Limit
0.02ng/L
HOLDING TIME
Holding times for extraction were exceeded for all samples by approximately 60
days. However, all samples were stored at 4°C preventing biodegradation of
the samples. All samples were analyzed within 40 days of extraction, which
meets the established criteria.
DETECTION LIMITS Detection limits ranged from 0.007 to 0.07 ng/L. The higher detection limits
were associated with samples requiring dilution or those with high PAH
concentrations that required smaller extraction volumes.
METHOD BLANKS
MATRIX SPIKES
REPLICATES
SRMS
SURROGATES
One method blank was analyzed with the samples. The blank was free of PAH
compounds except Naphthalene and benzo(ghi)perylene were detected at
levels near detection limits in the blank. These levels were less than five times
the levels found in all but three samples. Surrogate recoveries in the blanks
ranged from 61 to 67%.
One sample was spiked in duplicate for PAHs. The matrix spike recoveries
were all negative percentages except for Benzo(a)anthracene (2026%),
benzo(k)fluoranthene (84%) and dibenzo(a,h)anthracene (4%). The
concentration of the spike was generally much lower than the sample
concentration, causing difficulty in detecting the spike signal. The spike
duplicate showed recoveries ranging from 3 to 197% with a negative recovery
for benzo(b)fluoranthene. This indicates some matrix interference.
One sample was extracted and analyzed in triplicate. Relative standard
deviations were generally between 25 and 35%. Dibenzo(a,h)anthracene RSD
was 47%. Naphthalene, acenaphthalene and acenaphthene had RSDs below
20%, which is within the established criteria.
SRMs are not available for PAHs in water.
Most surrogates were outside the established criteria, probably due to matrix
interference and high sample concentrations relative to surrogate
concentrations used.
1 6
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polychlorinated biphenyls (PCBs)
Batteile Marine Science Laboratories
Water
SAMPLE NUMBER: 23
Reference
Method
MSL-M-41
Range of
Recovery
40-120%
Relative
Precision
+20%
Detection
Limit
HOLDING TIME
Holding times for extraction were exceeded for all samples by approximately 60
days. However, all samples were stored at 4°C preventing biodegradation of
the samples. All samples were analyzed within 40 days of extraction, which
meets the established criteria.
DETECTION LIMITS The detection limits ranged from 0.05ng/L to 0.2 ng/L for undiluted samples and
from 0.5ng/L to 2jxg/L for diluted samples.
METHOD BLANK
MATRIX SPIKE
REPLICATES
SURROGATES
One method blank was prepared and analyzed with the samples. No PCBs
were detected in the blank. Surrogate recoveries were 62 and 96% in the
blank.
One matrix spike was prepared and analyzed with the samples for Aroclor
1254. The recovery was 112% and the surrogate recoveries were 44 and 50%.
A duplicate spike was set up but was not spiked.
One sample was extracted and analyzed in triplicate with an BSD of 41%.
Most samples were within the criteria for surrogate recovery of 40 to 120%.
Seven of 23 samples had one surrogate recovery outside the required criteria.
Both surrogate recoveries for 1 sample were below the required criteria.
17
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polynuclear Aromatic Hydrocarbons (PAHs)
Battelle Marine Science Laboratories
Sediments
SAMPLE NUMBER: 97
Reference
Method
MSL-M-42
Range of
Recovery
40-120%
Relative
Precision
±20%
Detection
Limit
0.02ng/Kg
HOLDING TIMES
Samples were held frozen up to 3 months prior to extraction and most were
analyzed within the EPA extract holding time of 40 days (EPA 1986).
DETECTION LIMITS Detection limits ranged from 0.004 to 0.053 ng/g.
METHOD BLANKS
MATRIX SPIKES
SRMs
REPLICATES
SURROGATES
Seven method blanks were extracted and analyzed for PAHs; one with each
batch of samples. PAHs were not detected in the blanks.
Eight samples were spiked in duplicate with a known concentration of PAH
standard. One sample had suspect results and was re-analyzed. However, the
spikes were not re-analyzed with it, therefore, that data has not been included.
A second sample had suspect results and was rerun along with the spikes. The
rerun results were reasonable and have been included in the data package.
For the 17 PAH compounds analyzed, spike 379GLBRM11 had recoveries
within the 40-120% criteria and the duplicate spike had 4 compounds within the
criteria. The spike 379GLBR*247 had 12 of 17 and the duplicate had 10 of 17
compounds within the. Both the spike 379GLBR*247 (rerun) and the duplicate
had 14 of 17 compounds within the criteria. The spike 379GLBR*268 had 8 of
17 and the duplicate had 16 of 17 compounds within the criteria. Both the spike
379GLBR*388 and the duplicate had 12 of 17 compounds within the criteria.
The spike 379GLBR*388 (rerun) had 14 of 17 and the duplicate had 13 of 17
compounds within the criteria.
SRMs certified for PAHs in sediments are not available.
Five samples were extracted and analyzed in triplicate. Of those triplicates, one
had 17 of 17 compounds within the ±20 criteria, two had 14 of 17 and two had
11 of 17 within the criteria. Those compounds with higher RSDs were
associated with low concentrations near the detection limits.
Four surrogates were added to all samples. Of the 97 samples analyzed, 41
had one surrogate outside the recovery criteria of 40-120%, 8 had two
surrogates outside the criteria and 2 had three surrogates outside the criteria.
1 8
-------
QA/QC SUMMARY
PROGRAM:
PARAMETER:
LABORATORY:
MATRIX:
Buffalo River Pilot Project
Polychlorinated biphenyls (PCBs)
Battelle Marine Science Laboratories
Sediments
SAMPLE NUMBER: 46
Reference
Method
MSL-M-42
Range of
Recovery
40-120%
Relative
Precision
±20%
Detection
Limit
0.02u.g/Kg
HOLDING TIMES Samples were held frozen for up to 3 months prior to extraction and were most
were analyzed within the EPA extract holding time of 40 days (EPA 1986).
DETECTION LIMITS Detection limits ranged from 0.025 to 0.060n.g/Kg.
METHOD BLANKS One method blank was extracted and analyzed with each batch. No PCBs were
detected in the blanks.
MATRIX SPIKES
SRMs
REPUCATES
SURROGATES
One sample was spiked with Aroclor 1254. Four samples were spiked in
duplicate with Aroclor 1254. Three of the seven recoveries were within the
criteria of 40-120%.
Only one SRM is certified for PCBs in sediments, which is HS-2 from the
National Research Council of Canada. However, only Aroclor 1254 is certified
for packed column chromatography. We used capillary column chromatography.
Therefore, no certified SRMs are available for PCBs in sediment using the method
we follow.
Two samples were extracted and analyzed in triplicate. Sample 379GLBFT199
had an RSD for Aroclor 1254 of 89%, and an RPD of 117% for Aroclor 1248.
The second replicate, 379GLBR*323 had RSDs within the criteria for all
compounds.
Two surrogates were added to each sample. Thirty-three of 46 samples had one
surrogate outside the criteria of 40-120%. Thirty-two of those 33 samples
were outside the criteria because the amount of surrogate octachloronaphthalene
added was too low relative to the sample concentrations and was difficult to
resolve.
1 9
-------
BUFFALO RIVER PILOT PROJECT (CF* 379)
DOXINS/FURANS IN AIR SAMPLES
(Concentrations In no/sample)
MSLCode
379GLBR-112ABE
379GLBR-112F
379GLBR-232ABD
379GLBR-233ABD
379GLBR-234ABD
379GLBR-272ABD
Sponsor ID
22OCT5:0011GA10
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5-.3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
2378-
TCDF
0.086 U
0.057
0.037
0.000
0.059
0.380
TOTAL
TCOF
0.100
0.260
0.480
0.830
1.100
3.800
2378-
TCDO
0.079 U
0.027 U
0.036
0.041
0.021
0.089
TOTAL 1
TCDO
NA
NA U
0.290
0.400
0.210
1.100
2378-
PeCDF
0.033
0.031
0.040
0.057
0.055
0.360
23478-
PeCDF
0.056 U
0.048
0.056
0.087
0.063
0.340
TOTAL
PeCDF
0.380
0.400
0.530
1.200
0.840
3.700
12378-
PeCDO
0.330
0.023 U
0.079
0.086
0.036 U
0.180 U
TOTAL 123478- 123678-
PeCDF HxCDF HxCDF
0.320
0.150
0.670
0.770
0.490
2.600
0.042
0.043
0.078
0.140 U
0.048
0.390
0.053
0.046
0.076
0.130
0.054
0.330
123789-
HxCDF
0.110
0.140
0.150
0.220
0.043
0.230
Method Blank
Method Blank
0.0260 U
NA 0.0530 U
NA 0.0120 U 0.0082 U
NA 0.0110 U
NA 0.0076 U 0.0094 U 0.0058 U
MATRIX SPIKE RESULTS
Spike
Quantity Spiked
Quantity Measured
Percent Recovery
Spike Duplicate
Quantity Spiked
Quantity Measured
Percent Recovery
NA - Not applicable.
* - Outside of Internal QC criteria (40-120%).
0.200
0.230
115%
0.200
0.240
120%
0.200
0.230
115%
0.200
0.240
120%
0.200
0.250
125% '
0.200
0.240
120%
0.200
0.250
125% *
0.200
0.240
120%
1.000
1.100
110%
1.000
1.100
110%
1.000
1.100
110%
1.000
1.200
120%
2.000
2.200
110%
2.000
2.300
115%
1.000
1.100
110%
1.000
1.100
110%
1.000
1.100
110%
1.000
1.100
110%
1.000
0.970
97%
1.000
0.960
96%
1.000
0.890
89%
1.000
0.930
93%
1.000
0.870
87%
1.000
0.930
93%
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF* 379)
DOXINS/FURANS IN AIR SAMPLES
(Concentrations In ng/sample)
MSLCode
379GLBR-112ABE
379GLBR-112F
379GLBR-232ABD
379GLBR-233ABD
379GLBR-234ABD
379GLBR-272ABD
234678-
Sponsor ID HxCDF
22OCT6:0011GA10
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5.-3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB30
0.076 U
0.042
0.028
0.054
0.023 U
0.044
TOTAL 123478- 123678- 123789-
HxCDF HxCDO HxCDO HxCDO
0.560
0.590
0.890
1.100
0.440
2.800
0.050
0.013 U
0.031
0.049
0.026 U
0.120
0.091
0.022
0.050
0.071
0.038 U
0.130
0.130
0.011 U
0.025
0.050
0.020
0.110
TOTAL 1234678- 1234789-
HxCDO HpCOF HpCDF
1.500
0.100
0.660
1.000
0.490
2.900
0.510
0.620
0.750
1.200
0.250
1.600
0.100
0.120
0.110
0.180
0.023
0.110
TOTAL 1234678-
HpCDF HpCDO
0.710
1.200
1.100
1.900
0.410
1.900
1.600
0.210
0.450
0.780
0.260
1.500
TOTAL
HpCDO
3.300
0.390
0.900
2.300
0.680
4.000
OCOF
1.300
1.600
1.000
1.600
0.160
0.650
OCOD
5.200
0.910
1.600
3.000
1.300
4.900
Method Blank
Method Blank
0.0077 U
MATRIX SPIKE RESULTS
Spike
Quantity Spiked
Quantity Measured
Percent Recovery
Spike Duplicate
Quantity Spiked
Quantity Measured
Percent Recovery
NA - Not applicable.
* - Outside of Internal QC criteria (40-120%).
NA 0.0083 U 0.0097 U 0.0120 U
1.000
0.980
98%
1.000
1.000
100%
4.000
3.700
93%
4.000
3.800
95%
NA
1.000
1.200
120%
1.000
1.200
120%
1.000
1.300
130% *
1.000
0.990
99%
1.000
1.200
120%
1.000
0.990
99%
3.000
3.700
123%
3.000
3.200
107%
0.0190 U 0.0077 U
1.000
1.100
110%
1.000
1.200
120%
NA
NA
NA 0.0210
1.000
1.600
160% *
1.000
1.600
160% *
2.000
2.700
135% *
2.000
2.800
140% *
1.000
0.970
97%
1.000
1.100
110%
1.000
0.970
97%
1.000
1.100
110%
2.000
2.300
115%
2.000
2.400
120%
2.000
2.100
1 05%
2.000
2.100
105%
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF« 379)
DOXINS/FURANS IN AIR SAMPLES
INTERNAL STANDARDS
% Recovery
MSLCode
Sponsor ID
2378-
TCOF
-C13
2378-
TCOO
-C13
12378-
PeCOF
-C13
23478-
PeCDF
-C13
12378- 123478- 1
PeCOO
-C13
HxCDF
-C13
23678- 123789- 234678-
HxCDF
-C13
HxCDF
-C13
HxCDF
-C13
123478-
HxCOD
-C13
123678-
HxCDD
-C13
379GLBR-112ABE 22OCT5:0011GA10
379GLBR-112F 22OCT5:0011GA10
379GLBR-232ABD 23OCT4:4511GA2O
379GLBR-233ABD 24OCT5:3011GA3O
379GLBR-234ABD 25OCT1:4511GB1O
379GLBR-272ABD 31OCT1:0011GB3O
Method Blank Method Blank
MATRIX SPIKE RESULTS
Spike (% Recovery)
Spike Duplicate (% Recovery)
NA - Not applicable.
' . Outside of Internal QC criteria (40-120%).
92
78
93
104
78
88
93
73
88
101
77
88
70
63
73
79
61
68
85
NA
111
103
113
100
66
37
42
62
40
37
106
NA
93
93
86
89
83
86
93
102
79
88
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA ..
NA
122
NA
115
145
115
148
72
80
83
89
73
73
85
81
75
80
84
71
73
77
60
124
103
109
57
46
36
96
94
90
92
88
82
NA
NA
NA
NA
NA
NA
120
130
106
77
72
75
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF« 379)
DOXJNS/FURANS IN AIR SAMPLES
% Recovery
MSLCode
379GLBR-112ABE
379GLBR-112F
379GLBR-232ABD
379GLBR-233ABD
379GLBR-234ABD
379GLBR-272ABD
Method Blank
Sponsor ID
22OCT5:0011GA10
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5:3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
Method Blank
1234678- 1234789-1234678-
HpCOF HpCDF UpCDD
-C13 -C13 -C13
77
69
74
82
64
70
76
119
NA
108
108
110
108
105
87
73
83
91
73
76
72
OCCO
-C13
102
61
83
95
59
74
59
1234- 123789-
TCDO HxCDD
-C13 -C13
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
2378-
TCDD
-C13
100
NA
99
101
99
95
100
METHOD BLANK RESULTS
Spike
Spike Duplicate
(% Recovery)
(% Recovery)
53
44
135
135
77
63
67
50
NA
NA
NA
NA
93
100
NA - Not applicable.
' - Outside of internal QC criteria (40-120%).
Page 4
-------
MATRIX: XAO
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
(Concentrations in ng/sampl&)
MSI Code Sponsor ID
379GLBR-112ABE 22OCT5:0011GA10
379GLBR-232ABD 23OCT4:4511GA2O
379GLBR-233ABD 24OCT5:3011GA3O
379GLBR-234ABD 25OCT1:4511G31O
379GLBR-272ABD 31OCT1:0011GB3O
Method Blank-XAD
MATRIX SPIKE RESULTS
Amount Spiked
Method Blank
Blank + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Method Blank
Blank + Spike Duplicate
Amount Recovered
Percent Recovery
Naph- Acenaph-
thalene thylene
155261 BD(1)
19086 BD(2)
13944 BD(2)
8922 B0(2)
111623 80(1)
77
1500
77
1137
1060
71%
1500
77
1573
1496
100%
75290
82
168
187
541 0
60U
1500
60 U
1097
1097
73%
1500
60 U
1401
1401
93%
Acenaph-
thene Flourene
148970(1)
305
414
478
16630
60 U
1500
60U
1395
1395
93%
1500
60U
1973
1973
132% *
6766 D
448
470
854
3841 D
60 U
1500
60 U
1154
1154
77%
1500
60 U
1662
1662
111%
Phenan-
threne
51605D(i)
3568 0(2)
4044 0(2)
3743 0(2)
44750 0(1)
60U
1500
60 U
1159
1159
77%
1500
60 U
1615
1615
108%
Anthra-
cene
54920
330
477
813
44230
60U
1500
60 U
957
957
64%
1500
60 U
1324
1324
88%
Fluoran-
thena
12605 D
1289
1650
1779 0(2)
321870(1)
60 U
1500
60 U
1381
1381
92%
1500
60 U
1962
1962
131% *
Pyrene
22876D(i)
728
1296
2691
11 9450
60U
1500
60U
1211
1211
81%
1500
60 U
1689
1689
113%
# - All benzofluoranthene isomers (b, j & k) are quantified together
B • Analyte was also detected in the associated blank
D - Secondary analysis performed at dilution factor of 1:5
D(1) • Third analysis performed at dilution factor of 1:100
0(2) - Secondary analysis performed at dilution factor of 1:20
U • Undetected at the given method detection limit
* - Outside EPA and internal QC criteria (40-120%).
-------
MATRIX: XAD
(Concentrations in ng/sample)
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
Benz[a]-
MSLCode Sponsor ID anthracene
379GLBR-1 1 2ABE 22OCT5:001 1 GA1 0
379GLBR-232ABD 23OCT4:4511GA2O
379GLBR-233ABD 24OCT5:3011GA3O
379GLBR-234ABO 25OCT1:4511GB1O
379GLBR-272ABD 31 OCT1 :001 1 GB3O
Method Blank-XAD
MATRIX SPIKE RESULTS
Amount Spiked
Method Blank
Blank + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Method Blank
Blank + Spike Duplicate
Amount Recovered
Percent Recovery
54520 D
128
268
946
5011 D
60U
1500
60 U
1225
1225
82%
1500
60 U
1708
1708
114%
Benzofluor-
Chrysene anthenes #
5370 D
159
286
699
3629 D
60 U
1500
60 U
1153
1153
77%
1500
60 U
1579
1579
105%
26060
313
363
839
6656 D
120U
1500
120U
2611
2611
87%
1500
120U
3749
3749
125% *
Indeno
Benzo[a]- [1,2,3-cd]- Dibenz[a,h)- Benzo[ghi]
pyrene pyrene anthracene perylene
2956 D
69
124
223
8050
60 U
1500
60U
804
804
54%
1500
60 U
1000
1000
67%
711 D
60 U
64
214
1234 D
60 U
1500
60U
1292
1292
86%
1500
60 U
1812
1812
121% *
6660
60 U
60 U
60 U
60U
60 U
*
1500
60 U
1331
1331
89%
1500
60U
1852
1852
123% *
3118D
77
97
121
4340
60U
1500
60 U
1215
1215
81%
1500
60 U
1678
1678
112%
# - All benzofluoranthene isomers (b, j & k) are quantified together
B - Analyte was also detected in the associated blank
D m Secondary analysis performed at dilution factor of 1:5
D(1) - Third analysis performed at dilution factor of 1:100
D(2) • Secondary analysis performed at dilution factor of 1:20
U • Undetected at the given method detection limit
' • Outside EPA and internal QC criteria (40-120%).
Page 2
-------
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
MATRIX: XAD
MSLCode Sponsor ID
379GLBR-112ABE 22OCT5:0011GA10
379GLBR-232ABD 23OCT4:4511GA2O
379GLBR-233ABD 24OCT5:301 1 GA3O
379GLBR-234ABD 25OCT1:4511GB1O
379GLBR-272ABD 31OCT1:0011GB3O
Method Blank-XAD
MATRIX SPIKE RESULTS
Amount Spiked
Method Blank
Blank + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Method Blank
Blank + Spike Duplicate
Amount Recovered
Percent Recovery
% Surrogate Recovery
D10- D10- 010-
Fluorene Anthracene Pyrene
162% D * 107% D 204% D *
60% 66% 65%
58% 63% 67%
108% 113% 116%
94% 0 101% D 111%D
103% 79% 109%
NA NA NA
103% 79% 109%
77% 63% 86%
NA NA NA
NA NA NA
NA NA NA
103% 79% 109%
107% 87% 120%
NA NA NA
NA NA NA
# - All benzofluoranthene isomers (b, j & k) are quantified together
B • Analyte was also detected in the associated blank
D • Secondary analysis performed at dilution factor of 1:5
0(1) • Third analysis performed at dilution factor of 1:100
0(2) » Secondary analysis performed at dilution factor of 1:20
U - Undetected at the given method detection limit
* - Outside EPA and internal QC criteria (40-120%).
Page 3
-------
MATRIX: WATER
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
MSLCoda
379GLBR-112CD
379GLBR-232C
379GLBR-233C
379GLBR-234C
379GLBR-272C
Sponsor ID
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5:3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
Naph-
thalene
299
98
56
92
93
Acenaph- Acenaph-
thylene
41
45U
sou
57 u
74 U
thene
103
45u
SOU
57 U
74U
Flourene
123
45 U
50 U
57 u
74 U
Phenan-
threne
2975 D
61
55
96
74 U
Anthra-
cene
233
45U
SOU
57 U
74 u
Fluoran-
thene
14330
45U
SOU
187
74 u
Pyrene
4602 D
46
55
186
74 U
Method Blank-WATER
20 u
20u
20 U
20 u
20 U
20U
20 U
20 U
MATRIX: SOLVENT BLANK
MSLCode
Sponsor ID
Naph-
thalene
Acenaph-
thylene
Acenaph-
thene
Flourene
Phenan-
threne
Anthra-
cene
Fluoran-
thene
Pyrene
379GLBR-112F 22OCT5:0011GA10 4571 B
400 U
633
1472
10686
400 U
2544
1132
# • All benzofluoranthene isomers (b, j & k) are quantified together
B m Analyte was also detected in the associated blank
D • Secondary analysis performed at dilution factor of 1:5
U - Undetected at the given method detection limit
I • Interference present
* - Outside EPA and internal QC criteria (40-120%).
Page 4
-------
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
MATRIX: WATER
(Concentrations in ng/L)
MSLCode
379GLBR-112CD
379GLBR-232C
379GLBR-233C
379GLBR-234C
379GLBR-272C
Sponsor ID
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5:3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
Method Blank-WATER
MATRIX: SOLVENT BLANK
MSLCode
Sponsor ID
Benz[a]-
anthracene
647
45
50
57
74
20
u
u
u
u
u
(Concentrations
Benz[a]-
anthracene
Chrysene
890
45U
SOU
57 U
74 u
20 U
in ng/L)
Chrysene
Benzofluor-
anthenes #
235
91 U
100U
114 U
148U
40U
Benzofluor-
anthenes *
Benzo(a]-
pyrene
149
45
50
57
74
20
Benzo[a]-
pyrene
u
u
u
u
u
Indeno
[1,2.3-cd]-
pyrene
57
45 u
50 u
57 U
74 U
20 U
Indeno
[1,2,3-cd]-
pyrene
Dibenzja.h]-
anthracene
70
45
50
57
74
20
Dibenz[a,h]-
anthracene
u
u
u
U
u
Benzo[ghi]
perylene
170
45u
sou
57u
74 U
20 u
Benzo(ghi)
perylene
379GLBR-112F 22OCT5:0011GA10
400 U
400 u
800 u
400 U
400 U
# • All benzofluoranthene isomers (b, j & k) are quantified together
B - Analyte was also detected in the associated blank
D • Secondary analysis performed at dilution factor of 1:5
U • Undetected at the given method detection limit
I - Interference present
* - Outside EPA and internal QC criteria (40-120%).
400 u
400 u
PageS
-------
MATRIX: WATER
379GLBR-112CD
379GLBR-232C
379GLBR-233C
379GLBR-234C
379GLBR-272C
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5:3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
BUFFALO RIVER PILOT PROJECT (#379)
SIR/PAH ANALYSIS
IN AIR SAMPLES
MSLCode
Sponsor ID
% Surrogate Recovery
D10- D10-
Fluorene Anthracene
D10-
Pyrene
Method Blank-WATER
89%
74%
52%
75%
69%
52%
85%
79%
54%
71%
65%
35%*
149% )
89%
68%
87%
87%
72%
MATRIX: SOLVENT BLANK
MSLCode
Sponsor ID
% Surrogate Recovery
D10- D10-
Fluorene Anthracene
D10-
Pyrene
379GLBR-112F 22OCT5:0011GA10
101%
80%
116%
# - All benzofluoranthene isomers (b, j & k) are quantified together
B • Analyte was also detected in the associated blank
D - Secondary analysis performed at dilution factor of 1:5
U • Undetected at the given method detection limit
I - Interference present
* - Outside EPA and internal QC criteria (40-120%). .
Page 6
-------
BUFFALO RIVER PILOT PROJECT (#379)
PCB/PESTICIDE ANALYSIS
IN AIR SAMPLES
MATRIX: XAD
(Concentrations in ug/sample)
MSLCode Sponsor ID
379GLBR-112ABE 22OCT5:0011GA10
379GLBR-232ABD 23OCT4:451 1 GA2O
379GLBR-233ABD 24OCT5:301 1 GA3O
379GLBR-234ABD 25OCTV.4511GB1O
379GLBR-272ABD 31OCT1:0011GB3O
Method Blank-XAD
MATRIX SPIKE RESULTS
Amount Spiked
Method Blank
Blank + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Method Blank
Blank + Spike Duplicate
Amount Recovered
Percent Recovery
MATRIX: SOLVENT BLANK
MSLCode Sponsor ID
Monochloro-
biphenyl
0.75 U
0.75 U
0.75 U
0.75 U
0.75 U
0.75 U
12
0.75 U
6.6
6.6
55%
12
0.75 U
7.3
7.3
61%
(Concentrations
Monochloro-
biphenyl
Dichloro-
biphenyl
0.75 U
0.75 U
0.75 U
0.75 U
0.75 U
0.75 U
12
0.75 U
7.8
7.8
65%
12
0.75 U
7.7
7.7
64%
in ug/L)
Dlchloro-
biphenyl
Trlchloro-
biphenyl
0.75
0.75
0.75
0.75
3.6
0.75
12
0.75
8.7
8.7
73%
12
0.75
7.8
7.8
65%
Trichloro-
biphenyl
Tetrachloro-
biphenyl
U 1.5
U 1.5
U 1.5
U 1.5
2.3
U 1.5
24
U 1.5
18
18
75%
24
U 1.5
16
16
67%
Tetrachloro-
biphenyl
Pentachloro-
biphenyl
U 1.5U
U 1.5 U
U 1.5U
U 1.5U
2.9
U 1.5 U
24
U 1.5U
17
17
71%
24
U 1.5 U
13
13
54%
Pentachloro-
blphenyl
Hexachloro-
biphenyl
1.5
1.5
1.5
1.5
1.5
1.5
24
1.5
18
18
75%
24
1.5
13
13
54%
Hexachloro-
biphenyl
Heptachloro-
biphenyl
U 2.3 U
U 2.3 U
U 2.3 U
U 2.3 U
U 2.3 U
U 2.3 U
36
U 2.3 U
27
27
75%
36
U 2.3 U
19
19
53%
Heptachloro-
biphenyl
Octachloro-
biphenyl
2.3 U
2.3 U
2.3 U
2.3 U
2.3 U
2.3 U
•
36
2.3 U
27
27
75%
36
2.3 U
19
19
53%
Octachloro-
blphenyt
379GLBR-112F 22OCT5:0011GA10
5.0 U
5.0 U
5.0 U
10U
10U
10 U
15U
15 U
> Undetected at the given method detection limit.
Outside EPA and Internal OC criteria (40-120%).
Page 1
-------
BUFFALO RIVER PILOT PROJECT (#379)
PCB/PESTICIDE ANALYSIS
IN AIR SAMPLES
MATRIX: XAD
MSLCode
Sponsor 10
(Concentrations in ug/sample)
Nonachloro- Decachloro-
biphenyl biphenyl
% Surrogate Recovery
2-Fluoro-
biphenyl
C13-Tetrachloro- C13-Octachloro-
biphenyl biphenyl
379GLBR-112ABE
379GLBR-232ABD
379GLBR-233ABD
379GLBR-234ABD
379GLBR-272ABD
Method Blank-XAD
22OCT5:0011GA10
23OCT4:4511GA2O
24OCT5:3011GA3O
25OCT1:4511GB1O
31OCT1:0011GB3O
MATRIX SPIKE RESULTS
Amount Spiked
Method Blank
Blank + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Method Blank
Blank + Spike Duplicate
Amount Recovered
Percent Recovery
2.3 U
2.3 U
2.3 U
2.3 U
2.3 U
2.3 U
3.8 U
3.8 U
3.8 U
3.8 U
3.8 U
3.8 U
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
60
3.8 U
45
45
75%
60
3.8 U
32
32
53%
62%
81%
77%
60%
53%
23%
NA
23%'
55%
NA
NA
NA
23%
64%
NA
NA
71%
107%
112%
94%
95%
67%
NA
67%
97%
NA
NA
NA
67%
71%
NA
NA
59%
96%
105%
92%
88%
64%
NA
64%
92%
NA
NA
NA
64%
67%
NA
NA
MATRIX: SOLVENT BLANK
MSLCode Sponsor ID
(Concentrations in ug/L)
Nonachloro- Decachloro-
biphenyl biphenyl
% Surrogate Recovery
2-Fluoro-
biphenyl
C13-Tetrachloro- C13-Octachloro-
biphenyl biphenyl
379GLBR-112F 22OCT5:0011GA10
15
25
47%
93%
94%
U « Undetected at the given method detection limit.
' > Outside EPA and internal QC criteria (40-120%).
Page 2
-------
PROJECT:
ISSUED TO:
tuuin citv testmcj
corporation
REPORT OF: CHEMICAL ANALYSES
662 CROMWELL AVENUE
ST. PAUL, MN 55114
PHONE 612/645-3601
PCB/PAH ANALYSES
Battelle Pacific Northwest Division
Attn: Ms. Linda Bingler
Marine Sciences Laboratory
439 West Sequim Bay Road
Sequim, WA 98382
DATE: January 9, 1992
INVOICE NO: 4410 92-0442B
INTRODUCTION
This report summarizes the results from analyses performed on eleven samples which were submitted by
a representative of Battelle Pacific Northwest Division. Six of the samples were analyzed for the presence
or absence of polychlorinated biphenyls (PCBs) using a modified version of USEPA Method 680 and all
of the samples were analyzed for polynuclear aromatic hydrocarbons (PAHs) using a version of USEPA
Method 8270 adapted for selected-ion-monitoring analyses.
SAMPLE IDENTIFICATION
Client ID
379GLBR*112ABE
379GLBR*112CD
379GLBR*112F
379GLBR*232ABD
379GLBR*232C
379GLBR*233ABD
379GLBR*233C
379GLBR*234ABD
379GLBR*234C
379GLBR*272ABD
379GLBR*272C
Sample Type
Air
Impinger
Blank Solvent
Air
Impinger
Air
Impinger
Air
Impinger
Air
Impinger
Analyses
PCB/PAH
PAH
PCB/PAH
PCB/PAH
PAH
PCB/PAH
PAH
PCB/PAH
PAH
PCB/PAH
PAH
TCTID
268734
268743
268741
268735
268744
268736
268750
268737
268751
268738
268752
AS A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES. ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS.
AND AUTHORIZATION FOR PUBLICATION Of STATEMENTS. (
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCB/PAH ANALYSES DATE: January 9, 1992
PAGE: 2 INVOICE NO: 4410 92-0442B
METHODOLOGY
Sample Extraction
The XAD-2 resin and filter from each air sample component set were combined in a Soxhlet extractor and
spiked with the following surrogate standard compounds:
ug Spiked
2-Fluorobiphenyl 30
"CrTetrachlorobiphenyl 9.6
"G.-Octachlorobiphenyl 9.6
^lo-Fluorene 1.5
^KrAnthracene 1.5
1.5
Each sample was extracted with methylene chloride and each extract was combined with the respective
train rinse solvent component The extracts were transfered to Kuderna-Danish flasks, concentrated to 3.0
mL, and split into three equal portions for PCB, PAH, and PCDD/PCDF analyses. (The results from the
PCDD/PCDF analyses were reported previously in TCT report #4410 92-0442A.) The PCB portions were
solvent exchanged to hexane and spiked with 10 ug of each of the following perdeuterated internal
standards:
'H,.-Phenanthrene
'HrChrysene
The impinger catch samples were spiked with 0.5 ug of each of the three perdeuterated PAH surrogates
listed above, extracted with methylene chloride in separatory funnels, and the extracts were concentrated
to 1.0 mL using Kuderna-Danish glassware. All of the final PAH extracts were then spiked with 0.5 ug of
each of the following perdeuterated internal standards:
2H8-Naphthalene
^Hu-Acenaphthene
^lo-Phenanthrene
2H]2-Perylene
i A MUTUAL PROTECTION TO CLIENTS THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAI PROPFRTY OF Ct IFNTq
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCB/PAH ANALYSES DATE: January 9, 1992
PAGE: 3 INVOICE NO: 4410 92-0442B
PCB Analyses
PCS analyses were performed according to a modified version of USEPA Method 680. A 1-uL aliquot of
sach sample extract was injected by autosampler onto a 30 m DB-5 capillary column in a Hewlett-Packard
Model 5890A gas chromatograph. The column exit was interfaced directly into the ion source of a VG
Frio-2 quadrupole mass spectrometer operating in the positive ion electron impact (El) ionization mode
at 70 eV. The GC/MS operating conditions for these analyses are listed in Table 1. Data were acquired
in the selected-ion-monitoring mode and processed using a VG 11-250J data system.
A five point initial calibration curve was generated by analyzing standard solutions containing the target
compounds at concentrations ranging from 0.5-125 ug/raL as shown in Table 2. Each solution contained
internal standards at fixed concentrations of 10 ug/mL Response factors were generated for each target
anah/te relative to the corresponding internal standard using the measured area responses for characteristic
ions and the known concentrations. Continuing calibration check standards were analyzed daily prior to
sample analysis in order to verify the validity of the initial calibration. All calculations were performed as
specified in Method 680. The specific ions that were monitored for quantitation and confirmation of the
PCB compounds are listed in Table 3.
PAH Analyses
Ihe PAH analyses were performed by selected-ion-monitoring (SIM) gas chromatography/mass
spectrometry (GC/MS) using procedures from USEPA Method 8270. 2-uL aliquots of the sample extracts
were injected by autosampler onto a 30 m DB-5 capillary column in a Hewlett-Packard Model 5890A gas
chromatograph. The column exit was interfaced directly into the ion source of a VG Trio-2 quadrupole
mass spectrometer operating in the positive ion electron impact (El) ionization mode at 70 eV. Data were
acquired in the selected-ion-monitoring mode and processed using a VG 11-250J data system. The GC/MS
operating conditions for these analyses are summarized in Table 1A.
A five point initial calibration curve was generated by analyzing standard solutions containing each of the
target anah/tes at levels ranging from 20-1000 ng/mL and the internal standards at fixed concentrations of
500 ng/mL as indicated in Table 2A Quantifications of the target compounds were performed by
XHnparing the integrated areas of the chromatographic peaks with those of the internal standards as
specified in Method 8270. Continuing calibration standard analyses were performed daily prior to sample
analyses in order to verify the validity of the initial calibration. The specific ions that were monitored for
the PAH analyses are listed in Table 3A.
* MUTUAL PROTECTION TO CLIENTS THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
o AUTHORIZATION FOR PUBLICATION OF STATEMENTS CONCLUSIONS ofi EXTRACTIONS FROM OR REGARDING OUR REPORTS is RESERVED PENDING OUR PRIOR WRITTEN APPROVAL
-------
REPORT OF: CHEMICAL ANALYSES
PROJECTS PCB/PAH ANALYSES . DATE: January 13, 1992
PAGE: 4 INVOICE NO: 4410 92-0442B
RESULTS
The results from the analyses are included in the following appendices:
Appendix A Chain of Custody Documentation
Appendix B PCB Sample Analysis Results
Appendix C PCB QA/QC Analysis Results
Appendix D PCB Sample Chromatograms
Appendix E PCB QA/QC Chromatograms
Appendix F PAH Sample Analysis Results
Appendix G PAH QA/QC Analysis Results
Appendix H PAH Sample Chromatograms and Raw Data
Appendix I PAH QA/QC Chromatograms and Raw Data
DISCUSSION
The recoveries of the surrogate compounds in the PCB samples fell within the 50-125% guidelines specific*
in Method 680, with the exception of the 2-Fluorobiphenyl recovery (47%) in sample 379GLBR*112F. Th<
designated range for the surrogate compounds in the PAH samples is 50-150% for at least two of the thre<
surrogates in each sample. All of the surrogate recoveries in the PAH samples fell within this range, will
the exception of the perdeuterated pyrene (227%) in sample 379GLBR*112ABE. This elevated recover
resulted from the presence of an interference in the sample extract that was not resolved from the
surrogate peak. However, since the remaining two surrogates in this sample were recovered at acceptable
levels, the recovery criteria were met and no corrective action was required. The only other deviation fron
the target QC ranges was that of the raw area count for the perdeuterated naphthalene internal standarc
in sample 379GLBR*272ABD, which was 269% of the value for the corresponding standard in the daih
continuing calibration analysis. (The target range for internal standard areas in the sample extracts is 50
200% of the daily continuing calibration values.) However, upon analysis of a dilution of this sample
extract, the naphthalene internal standard area fell into the acceptable range.
A laboratory method blank was prepared and analyzed with each sample extraction batch as part of oui
routine quality control/quality assurance procedures. The results, found at the beginnings of Appendices
C and G, show the blanks to be free of the target PCB and PAH analytes, with the exception of a trace
background level (77 nanograms) of naphthalene in the blank associated with the PAH portions of the aii
AS A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES. ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENT
AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS. CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPROVA
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCB/PAH ANALYSES DATE: January 9,1992
PAGE: 5 INVOICE NO: 4410 92-0442B
DISCUSSION (Continued)
samples. The naphthalene levels determined for the affected samples were all higher than the naphthale
level in the blank by 20 times or more. This indicates that the sample processing steps did not contribu
significantly to the levels reported for the samples. A low recovery was achieved for the 2-Fluorobipher
surrogate in the PCB blank due to inadvertent volatilization of this compound during the concentrate
steps. Since the entire sample was consumed in the extraction process, any reprocessing in order
improve the recovery was not possible. Also, the blank associated with the impinger samples exhibited
low recovery (35%) for the perdeuterated anthracene surrogate. Since good recoveries were achieved fi
the other two surrogates in this blank, no corrective action was required
Two laboratory quality control PCB/PAH spike samples were prepared with the air sample batch I
extracting aliquots of clean resin that had been fortified with native standard materials. The result
included in Appendices C and G, show that the spiked native compounds were recovered at levels rangin
from 52-132%, which are all within the 50-135% target ranges designated for these analyses.
REMARKS
The sample extracts will be retained for a period of 60 days from the date of this report and then discarde<
unless other arrangements are made. The raw mass spectral data will be archived on magnetic tape fo
a period of not less than one year. Questions regarding the data contained in this report may be addressee
to the authors at the numbers provided below.
TWIN CITY TESTING CORPORATION
Steven W. Hannan, Scientist David P. Zimmerman, Scientist
High Resolution Mass Spectrometry Low Resolution Mass Spectrometry
Approved by:
_G./l
s.
Charles V. Sueperj^pefvisor Susan D. Max, Director
Mass Spectrometry Laboratory Operations
SWH/DPZ/clj
5 A MUTUAL PROTECTION TO CLIENTS THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
NO AUTHORIZATION FOR PUBLICATION OF STATEMENTS
-------
tuuin citv cestinp
corporation
® 662 CROMWELL AVENUE
REPORT OF: CHEMICAL ANALYSES £££%!££!£
PROJECT: PCDD/PCDF ANALYSES DATE: January 6, 1992
ISSUED TO: Battelle Pacific Northwest Division INVOICE NO: 4410 92-0442A
Attn: Ms. Linda Bingler
Marine Sciences Laboratory
Sequim, WA 98382
INTRODUCTION ~~~~
This report summarizes the results from the analyses performed on six air samples which were submitted
by a representative of Battelle Pacific Northwest Division. The samples were analyzed for the presence
or absence of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) using
a modified version of EPA Method 23. Polychlorinated biphenyl (PCB) and polynuclear aromatic
hydrocarbons (PAH) data will be reported under separate cover.
SAMPLE IDENTIFICATION
Client ID ** Sample Type TCT ID
379GLBR*112ABE Air 268734
379GLBR*112F Blank 268741
379GLBR*232ABD Air 268735
379GLBR*233ABD Air 268736
379GLBR*234ABD Air 268737
379GLBR*272ABD Air 268738
** Samples and sample components were split as per instructions from Battelle personnel included in
Appendix A.
METHODOLOGY
PCDD/PCDF Extraction
The XAD-2 resin portion of each sample component set was spiked with isotopically-labeled PCDD/PCDF
internal standards (Table 1), combined with the filter, and placed in a Soxhlet extractor thimble. The train
rinse solvents containing paniculate were filtered and the filters were added to the respective Soxhlet
extractor thimbles. The filtrate was then concentrated in the Soxhlet flask and the Soxhlet charged with
methylene chloride. The sample components were extracted for eighteen hours and the methylene chloride
was removed and concentrated. The Soxhlet was then recharged with benzene and extracted for an
additional eighteen hours. One third of each of the methylene chloride and benzene extracts were then
AS A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY Oc CLIENT
AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPHOVA
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCDD/PCDF ANALYSES DATE: January 6, 1992
PAGE: 2 INVOICE NO: 4410 92-0442A
PCDD/PCDF Extraction (Continued)
combined and quantitatively transferred to Kuderna Danish concentrators, concentrated, and solvent
exchanged to hexane. The hexane extracts were then processed through the anah/te enrichment procedures
described below.
Analvte Enrichment for PCDD/PCDF Analyses
The extraction procedure often removes a variety of compounds, in addition to the PCDDs and PCDFs,
from the sample matrix Some of these compounds can directly interfere with the analyses while others
can overload the capillary column causing degradation in chromatographic resolution or sensitivity. The
anah/te enrichment steps described below were used to remove interferences from the extracts.
The extracts were diluted to 100 mL with hexane, transferred to separatory funnels, and washed with IN
sodium hydroxide, concentrated sulfuric acid, and distilled water. The hexane layers were concentrated to
1 mL and quantitatively transferred to liquid chromatography columns containing alternating layers of silica
gel, 44% concentrated sulfuric acid on silica gel, and 33% 1N sodium hydroxide on silica gel The columns
were eluted with 60 mL of hexane and each entire eluate was collected and concentrated, under a gentle
stream of dry nitrogen, to a volume of 1 mL.
The extracts were then fractionated on liquid chromatography columns containing 4 g of activated alumina.
The columns were eluted with 10 mL of hexane followed by 7 mL of 2.0% methylene chloride/hexane and
25 mL of 60% methylene chloride in hexane. The 60% methylene chloride/hexane fractions were
concentrated to 1 mL under a stream of dry nitrogen and applied to the tops of chromatography columns
containing 1 g of 5% AX-21 activated carbon on silica gel Each column was eluted with
cyclohexane/methylene chloride (50:50 V/V) and cyclohexane/methanol/benzene (75:20:5 V/V) in the
forward direction, and then with benzene in the reverse direction. Each benzene fraction was collected,
spiked with recovery standards (1,2,3,4-TCDD-13C,2 and l,2,3,7,8,9-HxCDD-13Ci2) and concentrated to a
final volume of 20 uL.
PCDD/PCDF Analyses
The extracts were analyzed for the presence of PCDDs and PCDFs using combined capillary column gas
chromatography/high resolution mass spectrometry (HRGC/HRMS). The instrumentation consisted of
a Hewlett Packard Model 5890 gas chromatograph and a VG Model 70SE high resolution mass
spectrometer. The capillary column was interfaced directly into the ion source of the mass spectrometer,
thus providing the highest possible sensitivity while minimizing degradation of the chromatographic
resolution.
AS A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPROVAL
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT! PCDD/PCDF ANALYSES DATE: Januaiy 6, 1992
PAGE: 3 INVOICE NO: 4410 92-0442A
PCDD/PCDF Analyses (Continued)
The mass spectrometer was operated in the electron impact ionization mode at a mass resolution of
10,000-11,000 (M/&M, 10 percent valley definition). This resolution is sufficient to resolve most
interferences, such as PCBs, thus providing the highest level of confidence that the detected levels of
PCDD/PCDF are not false positives resulting from interferences. Typical operating parameters for the
HRGC/HRMS analyses are summarized in Table 2.
The data were acquired by selected-ion-recording (SIR) monitoring the groups of ion masses described in
EPA method 23. The five groups corresponded to the tetrachlorinated through octachlorinated congener
classes. Each group contained three ion masses for the PCDDs (with the exception of TCDD which
contained two ion masses), two ion masses for the PCDFs, the corresponding ion masses from the two
isotopically labeled internal standards, and the ion mass characteristic of the polychlorinated diphenylether
(PCDPE) which, if present, could cause false responses in the dibenzofuran channels. The third PCDD
ion mass monitored in the pentachloro through octachlorodibenzo-p-dioxin groups prevented the possibility
of misinterpretation of a polychlorinated biphenylene isomer as a PCDD. The two ion masses monitored
for TCDD also fulfilled this purpose.
Each group of ion masses also contained a lock mass which was monitored during the analyses to detect
suppressive interferences. It is particularly important to detect this type of interference since it can cause
the quantification of congener class levels to be artificially high if it occurs during the elution of an internal
standard or low if it occurs during the elution of the native analytes.
The lock mass was also used by the data system to automatically correct the mass focus of the instrument
The data system determined the centroid of the lock mass during each data acquisition cycle and corrected
the mass focus of the analyte and internal standard ion masses to assure that the centers of the mass peaks
were being monitored
The criteria used to judge positive responses for the PCDD/PCDF isomer included:
- Simultaneous response at both ion masses of the PCDD or PCDF
- Signal to noise ratio equal to or greater than 2.5:1.0 for both ion masses
- Chlorine isotope ratio within 15% of the theoretical value
5 A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
MD AUTHORIZATION FOR PUBLICATION OF STATEMENTS. CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUF1 PRIOR WRITTEN APPROVAL
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT PCDD/PCDF ANALYSES DATE: January 6, 1992
PAGE: 4 INVOICE NO: 4410 92-0442A
PCDD/PCDF Analyses (Cont)
- Chromatographic retention time within -1 to +3 seconds of the authentic standards (where
applicable)
- Chromatographic retention times within elution windows determined from analyses of standard
mixtures
- Absence of simultaneous response between the PCDF and diphenylether ion traces
A list of the exact ion masses monitored for the determination of PCDD/PCDF isomers and the PCDP
interferences is presented in Table 3. Also included are the theoretical chlorine isotope ratios for the te
congener classes.
Quantification and Calculations
The PCDD/PCDF isomers were quantified by comparison of their responses to the responses of the labele
internal standards as described EPA Method 23. Relative response factors were calculated from analyse
of standard mixtures containing representatives of each of the PCDD/PCDF congener classes at fiv
concentration levels, and each of the internal standards at one concentration level, as shown in Table <•
The PCDD/PCDF response factors were calculated by comparing the sum of the responses from the tw
ion masses monitored for each chlorine congener class to the sum of the responses from the two io;
masses of the corresponding isotopically labeled internal standard. Table 5 shows the response factor a
each of the calibration levels as well as the average response factors and the relative percent deviation fo
each. The formula for the response factor calculation is:
Rf -An x Qis
Ais x Qn
where:
Rf = Response factor
An = Sum of integrated areas for native isomer
Qis = Quantity of labeled internal standard
Ais = Sum of integrated areas for labeled internal standard
Qn = Quantity of native isomer
5 A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY Of CLIENT!
MO AUTHORIZATION FOR PUBLICATION OF STATEMENTS. (
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCDD/PCDF ANALYSES DATE: January 6, 1992
PAGE: 5 INVOICE NO: 4410 92-0442A
Quantification and Calculations (Cent)
The levels of PCDD/PCDF in the samples were quantified using the following equation:
C - An x Qis
where:
C = Concentration of target isomer or congener class
An = Sum of integrated areas for the target isomer or congener class
Qis = Quantity of labeled internal standard added to the sample
Ais = Sum of integrated areas for the labeled internal standard
W = Sample weight, volume or area
Rf = Response factor
Each pair of ion mass peaks in the selected-ion-current chromatograms was evaluated manually to
determine if it met the criteria for a PCDD or PCDF isomer. Areas of all peaks exhibiting correct ion
ratios and having retention times within the correct windows were then summed for calculations of total
congener concentrations. A summary of the high resolution initial calibration chlorine isotope ratios is
presented in Table 6. The toxic equivalency factors used to calculate the 2,3,7,8-TCDD equivalency are
listed in Table 7.
A limit of detection (LOD) based on producing a signal that is 2.5 times the noise level, was calculated for
each undetected 2,3,7,8-substituted isomer of any tetra through octa chlorinated congener class. The noise
heights used to calculate the detection limits were measured at the retention time of the specific isomer.
The formula used for calculating the LOD is:
LOD = Hn x Qis x 2.5
His x W x Rf
where:
LOD=Single isomer limit of detection
Hn =Sum of noise heights at native isomer retention time
Qis =Quantity of labeled internal standard added to the sample
His =Sum of peak heights for labeled internal standard
W = Sample weight, volume or surface area
Rf = Response factor
AS A MUTUAL PROTECTION TO CLIENTS THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY Of CLIENTS
AND AUTHORIZATION fon PUBLICATION OF STATEMENTS CONCLUSIONS OH EXTRACTIONS FROM on REGARDING OUR REPORTS is RESERVED PENDING OUR PRIOR WRITTEN APPROVAL
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCDD/PCPF ANALYSES . DATE: January 6, 1992
PAGE: 6 INVOICE NO: 4410 92-0442A
Quantification and Calculations (Cont)
The recovery of the 2,3,7,8-TCDD-ra4 enrichment efficiency standard and each 13C,2-labeled intern!
standard, relative to either 1,2,3,4-TCDD-13Q2 or l,2,3,7,8,9-HxCDD-13C12, was calculated using th
following equation:
%R = AJS x Ors x 100%
Rfr x Ars x Qis
where:
%R = Percent recovery of labeled internal standard
Ais = Sum of integrated areas of labeled internal standards
Qrs = Quantity of recovery standard
Ars = Sum of integrated areas of recovery standard
Rfr = Response factor of the specific labeled internal standard relative to the recovery standard
Qis = Quantity of the labeled internal standard congener added to the sample
RESULTS
Sample analysis results are included in the following:
Appendix A - Chain of Custody Documentation
Appendix B - Sample Analysis Results
Appendix C - QA/QC and Daily Calibration Results
Appendix D - Sample Chromatograms and Raw Data
Appendix E - Standard Chromatograms and Raw Data
Appendix F - QA/QC Chromatograms and Raw Data
DISCUSSION
The recoveries of the isotopically-labeled PCDD/PCDF internal and surrogate standards in the air sample:
generally ranged from 70-130%, indicating a high level of efficiency through the extraction and enrichmen
steps. Somewhat lower recovery values were obtained for selected internal standards in each of the
samples, many due to the presence of interfering substances in the final sample extracts. These
interferences, evidenced by suppressions in the lock mass ion traces, caused short-term fluctuations in the
AS A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY Of CLIENT:
AND AUTHORIZATION FOR PUBLICATION Of STATEMENTS CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPROVA
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCDD/PCPF ANALYSES DATE: January 6, 1992
PAGE: 7 . INVOICE NO: 4410 92-0442A
DISCUSSION (Continued)
sensitivity of the mass spectrometer, thereby decreasing the apparent recoveries for the affected standards.
(Actual recoveries are typically consistent throughout a given sample or show gradual trends instead of
abrupt changes.) All of the recoveries were, however, within the target ranges specified in the method, with
the exceptions of the labeled 1,2,3,7,8-PeCDD in samples 379GLBR*112F (37%), 379GLBR*272ABD
(37%), and the lab spike duplicate (36%). Also, slightly elevated recoveries were obtained for selected
surrogate compounds in samples 379GLBR*233ABD (labeled 1,2,3,4,7,8-HxCDD, 145%),
379GLBR*272ABD (labeled 1,2,3,4,7,8-HxCDD, 148%), the laboratory spike (labeled 1,2,3,4,7,8,9-HpCDF,
135%), and the laboratory spike duplicate (labeled 1,2,3,4,7,8,9-HpCDF, 135%). The native 1,2,3,7,8-
PeCDD concentrations should be accurate for these samples since quantitation is based on isotope dilution.
The native 1,2,3,4,7,8-HxCDD and 1,2,3,4,7,8,9-HpCDF concentration values in these four samples may,
however, be slightly elevated since both the native and surrogate isomers are compared to a separate
labeled isomer.
A laboratory method blank was prepared and analyzed with the sample extraction batch as part of our
routine quality control/quality assurance procedures. The data, included at the beginning of Appendix C,
show the blank to be free of PCDDs and PCDFs, with the exceptions of trace background levels of PeCDD
(19 picograms), HpCDD (6.3 picograms), and OCDD (92 picograms). The levels determined for the
affected isomers in the actual samples were higher than the corresponding blank levels by 3-100 times. It
should be noted, however, that levels less than five times higher than the background are not generally
considered to be statistically different from the background.
Two quality control PCDD/PCDF spike samples were also prepared with the sample batch by extracting
clean resin that had been fortified with native standard materials. The data, included in Appendix C, show
that the spiked native compounds were recovered at levels ranging typically from 87-130%. The only
compound with recoveries outside of this range was 1,2,3,4,7,8,9-HpCDF, which exhibited a recovery of
160% in each of the spike samples. It should be noted, however, that quality control ranges for native
spike sample recoveries are not specified in the method.
AS A MUTUAL PROTECTION TO CLIENTS, THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
AND AUTHORIZATION FOR PUBLICATION OF STATEMENTS CONCLUSIONS OR EXTRACTIONS FROM OR REGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPROVAL
-------
REPORT OF: CHEMICAL ANALYSES
PROJECT: PCDD/PCDF ANALYSES DATE: January 6, 1992
PAGE: 8 INVOICE NO: 4410 92-0442A
REMARKS
The sample extracts will be retained for a period of 60 days from the date of this report and then discarded
jnless other arrangements are made. The raw mass spectral data will be archived on magnetic tape for
i period of not less than one year. Questions regarding the data contained in this report may be addressed
:o the authors at the numbers provided below.
CITY TESTING CORPORATION
Steven W. Hannan, Scientist Charles V. Sueper, Supervisor
•iigh Resolution Mass Spectrometry Mass Spectrometry
;612)659-7336 (612)659-7520
Susan D. Max, Director
L-aboratory Operations
;612)659-7501
SWH/CVS/SDM/lml
A MUTUAL PROTECTION TO CLIENTS. THE PUBLIC AND OURSELVES ALL TWIN CITY TESTING CORPORATION REPORTS ARE SUBMITTED AS THE CONFIDENTIAL PROPERTY OF CLIENTS
J AUTHORIZATION FOR PUBLICATION OF STATEMENTS CONCLUSIONS OR EXTRACTIONS FROM OR FIEGARDING OUR REPORTS IS RESERVED PENDING OUR PRIOR WRITTEN APPROVAL
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN WATER SAMPLES
MSLCODE
379GLBR- 1 28 Rep 1
379GLBR- 1 28 Rep 2
379GLBR- 1 28 Rep 3
379GLBR- 1 32
379GLBR- 1 63
379GLBR- 165
379GLBR- 204
379GLBR- 187
379GLBR- 226
379GLBR- 227
379GLBR- 254
379GLBR- 255
379GLBR- 286 Rep 1
379GLBR- 286 Rep 2
379GLBR- 286 Rep 3
379GLBR- 326
379GLBR- 331
379GLBR- 361
379GLBR- 366
379GLBR- 370
379GLBR- 398
379GLBR 404
SPONSOR ID
I BIN A
23OCT4:459LA2O
23OCT4:459LA2O
23OCT4:459LA2O
23OCT5:2010LA2O
25OCT1 0:201 OLA3M
25OCT10:009LA3C
30OCT4:196LA3O
BIN B
25OCT3:0710LB1O
31OCT10:129LB2O
31OCT10:2110LB2O
31OCT2:5710LB3M
31OCT3:069LB3M
BIN C
18NOV5:559LC1O
18NOV5:559LC1O
18NOV5:559LC1O
19NOV5:509LC2O
19NOV5:0510LC2O
20NOV2:193LC3O
20NOV2:419LC3O
20NOV3:0110LC3O
BIN D
21NOV3:2610LD1O
21NOV4:169LD1O
DILUTION WATER
OIL & GREASE
(mg/L)
284.0
287..0
271.0
109.5
214.0
112.0
1.1 U
28.5
62.0
69.5
25.0
44.0
72.4
95.2
102.4
81.5
30.4
2.0
112.8
16.3
71.2
57.0
379GLBR- 275
6NOV12:003LO
1.1 U
U - Analyte detected below detection limits.
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN WATER SAMPLES
MSLCODE
SPONSOR ID
OIL & GREASE
(mg/L)
BLANKS
BLANK-1
BLANK-2
BLANK-3
BLANK-4
BLANK-5
BLANK-6
BLANK-7
BLANK'S
0.12
0
0
0.67
0
0
0.80
0
MATRIX SPIKE RESULTS
% RECOVERY
379GLBR- 128 * 23OCT4:459LA2O
379GLBR- 1 28 MATRIX SPIKE
379GLBR- 1 28 MATRIX SPIKE DUPLICATE
280.7
347.5
335.0
134% *
109%
379GLBR- 132 23OCT5:2010LA2O
379GLBR- 1 32 MATRIX SPIKE
379GLBR- 132 MATRIX SPIKE DUPLICATE
109.5
157.5
157.0
96%
95%
REPLICATE ANALYSES
379GLBR- 1 28 Rep 1
379GLBR- 1 28 Rep 2
379GLBR- 128 Rep 3
379GLBR- 286 Rep 1
379GLBR- 286 Rep 2
379GLBR- 286 Rep 3
23OCT4:459LA2O
23OCT4.-459LA2O
23OCT4:459LA2O
18NOV5:559LC10
18NOV5:559LC10
18NOV5:559LC10
RSD %
RSD %
284.0
287.0
271.0
3%
72.4
95.2
102.4
17%
U - Analyte detected below detection limits.
* - Mean of replicated sample.
" - Outside of QC criteria (40-120%).
RSD % = Relative Standard Deviation.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
MSLCODE
379GLBR- 1 3
379GLBR- 1 6
379GLBR- 1 7
379GLBR- 57
379GLBR- 58
379GLBR- 59
379GLBR- 104
379GLBR- 107
379GLBR- 108
379GLBR- 111 Rep 1
379GLBR- 111 Rep 2
379GLBR- 111 Rep 3
379GLBR- 113
379GLBR- 122
379GLBR- 123
379GLBR- 124
379GLBR- 136
379GLBR- 139
379GLBR- 141
379GLBR- 143
379GLBR- 145
379GLBR- 151
379GLBR- 152
379GLBR- 153
379GLBR- 166
379GLBR- 167
U = Analyte detected
R = Reruns.
SPONSOR ID
| BIN A
07OCT12:341SAO
07OCT1 2:401 SAO
07OCT1 2:091 SAO
09OCT11:502SA3O
09OCT1 1 :382SA2O
090CT11:282SA1O
22OCT11:317SA1O
22OCT11:378SA1O
22OCT4:203SA2O
220CT5:563SA2O
22OCT5:563SA2O
22OCT5:563SA2O
23OCT1 :303SA2O
23OCT4:284SA20
23OCT4:274SA2O
23OCT4:294SA2O
24OCT10:457SA2O
24OCT10:508SA2O
24OCT2:203SA3O
24OCT5:503SA3O
24OCT6:203SA30
25OCT9:224SA3O
25OCT9:224SA3O
25OCT9:214SA3O
25OCT9:307SA3O
25OCT9:368SA3O
below detection limits.
OIL & GREASE
ug/g
1211.6
1389.2
1644.3
1765.7
1819.5
1426.2
7232.5
3133.0
2565.5
2867.7
1839.4
2283.9
1855.0
94.6 U R
306.2 U R
300.9 U R
2390.8
696.4
1690.4
2669.4
2390.8
632.8 R
490.2 U
537.7 U
2442.7
1900.9
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
MSLCODE
379GLBR- 1 4
379GLBR- 21
379GLBR- 23
379GLBR- 65
379GLBR- 66
379GLBR- 67
379GLBR- 174
379GLBR- 176
379GLBR- 181
379GLBR- 182
379GLBR- 183
379GLBR- 193
379GLBR- 196
379GLBR- 198
379GLBR- 199 Rep 1
379GLBR- 199 Rep 2
379GLBR- 199 Rep 3
379GLBR- 206
379GLBR- 210
379GLBR- 213
379GLBR- 220
379GLBR- 221
379GLBR- 222
379GLBR- 242
379GLBR- 243
379GLBR- 244
379GLBR- 247
379GLBR- 248
379GLBR- 249
379GLBR- 268
379GLBR- 269 Rep 1
379GLBR- 269 Rep 2
379GLBR- 269 Rep 3
SPONSOR ID
| BIN B |
07OCT1:101SBO
07OCT1 2:531 SBO
07OCT1:011SBO
090CT9:542SB1O
09OCT10:152SB2O
09OCT10:352SB3O
25OCT12:153SB1O
25OCT2:153SB1O
25OCT2:254SB1O
25OCT2:294SB1O
25OCT2:284SB1O
25OCT3:527SB1O
25OCT3:578SB1O
30OCT2:493SB2O
30OCT4:013SB2O
300CT4:013SB2O
30OCT4:013SB2O
30OCT4:413SB2O
31OCT9:027SB2O
31OCT9:078SB2O
31OCT9:264SB2O
31OCT9:254SB2O
31OCT9:244SB2O
31OCT10:453SB3O
31OCT11:503SB3O
31OCT2.303SB3O
31OCT2:384SB3O
31OCT2:354SB3O
31OCT2:364SB3O
1NOV10:208SB3O
1NOV10:157SB3O
1NOV10:157SB3O
1NOV10:157SB3O
OIL & GREASE
ug/g
1144.5 R
1537.6
2174.0
2005.5
2082.0
1511.7
2357.2
1753.9 R
560.4 U
396.7 U
464.2 U
3770.7
1898.7
2071.2
1634.5
1306.0
1610.2 R
2148.9
1231.0
449.3
203.7
312.1
144.0 U
1192.5
1232.5 R
1549.8
235.9 U R
413.2 U
520.0 U
586.2 U
1436.9
1428.3
1633.9
U - Analyte detected below detection limits.
R «= Reruns.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
MSLCODE
379GLBR- 1 5
379GLBR- 1 8
379GLBR- 20
379GLBR- 73
379GLBR- 74
379GLBR- 75
379GLBR- 280
379GLBR- 282
379GLBR- 284
379GLBR- 288
379GLBR- 302
379GLBR- 303
379GLBR- 304
379GLBR- 307
379GLBR- 31 1
379GLBR- 313
379GLBR- 315
379GLBR- 323
379GLBR- 324
379GLBR- 325
379GLBR- 337
379GLBR- 340
379GLBR- 342
379GLBR- 344
379GLBR- 350
379GLBR- 351
SPONSOR ID
BIN C |
070CT1211SCO
07OCT1:331SCO
07OCT1:441SCO
09OCT4:562SC1O
09COT4:352SC2O
09OCT4:162SC3O
18NOV2:553SC1O
18NOV3:503SC1O
18NOV4:403SC1O
18NOV6:1510LC1O
19NOV8:594SC1O
19NOV9:004SC1O
19NOV9:014SC1O
19NOV9:238SC1O
19NOV11:303SC2O
19NOV2:203SC20
19NOV3:553SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV1:003SC3O
20NOV1:553SC3O
20NOV3 154SC3O
20NOV3 154SC3O
379GLBR- 352 20NOV3'154SC3O
379GLBR- 357 20NOV3.337SC3O
379GLBR- 360 Rep 1 20NOV3:278SC3O
379GLBR- 360 Rep 2 20NOV3.278SC3O
379GLBR- 360 Rep 3 20NOV3 278SC3O
OIL & GREASE
ug/g
2779.2
2180.1
1822.6
3995.4
1761.2
2398.5
2374.9 R
1845.4 R
2105.6 R
6290.3
527.6 U
786.6 R
371.5 U
2538.7
2729.1 R
1663.3
1641.1
507.7 U
471.6 U R
549.3 U
2416.0
4897.3
4759.8
3107.3
2695.4
4609.4
3549.0
4388.9
762.4
505.3 U
668.9 R
U = Analyte detected below detection limits.
R = Reruns.
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
MSLCODE
379GLBR- 1 9
379GLBR- 22
379GLBR- 24
379GLBR- 46
379GLBR- 51
379GLBR- 53
379GLBR- 376
379GLBR- 378
379GLBR- 380
379GLBR- 384 Rep 1
379GLBR- 384 Rep 2
379GLBR- 384 Rep 3
379GLBR- 388
379GLBR- 395
379GLBR- 396
379GLBR- 397
BLANK-1
BLANK-2
BLANK-3
BLANK-4
BLANK-5
BLANK-6
BLANK-7
BLANK-8
BLANK-9
SPONSOR ID
( BIN D
07OCT2:041SDO
07OCT1:521SDO
07OCT2.-122SDO
08OCT5:132SD3O
080CT5:402SD1O
08OCT5:302SD2O
21NOV12:003SD1O
21NOV1:353SD1O
21NOV2:433SD1O
21NOV5.078SD1O
21NOV5:078SD1O
21NOV5:078SD1O
21NOV5:107SD1O
21NOV5:224SD1O
21NOV5:224SD1O
21NOV5:224SD1O
OIL & GREASE
ug/g
2105.9
1342.1
1671.9
2347.2
2416.3
3038.9
3197.3 R
1054.8 R
2921.6 R
974.5
748.9
1172.9
5368.3
238.4 U
790.9
907.7
0.0060
0.0010
0.0020
0.0008
0.0020
0.0043
0.0033
0.0066
0.0000
U « Analyte detected below detection limits.
R = Reruns.
Page 4
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
OIL & GREASE
Ma CODE SPONSOR ID ug/g
MATRIX SPIKE RESULTS % RECOVERY
379GLBR- 111 * * 22OCT5:563SA2O 2330.3
379GLBR- 11 1 MATRIX SPIKE 3932.3 97%
379GLBR- 111 MATRIX SPIKE DUPLICATE 3369.5 82%
379GLBR- 182 25OCT2:294SB1O 610.OU
379GLBR- 182 MATRIX SPIKE 2190.7 158%
379GLBR- 182 MATRIX SPIKE DUPLICATE 2159.0 153%
379GLBR- 269 * * 1NOV10:157SB3O 1499.7
379GLBR-269 MATRIX SPIKE 2478.5 95%
379GLBR- 269 MATRIX SPIKE DUPLICATE 2533.9 91%
379GLBR- 360 * * 20NOV3:278SC30 645.5
379GLBR- 360 MATRIX SPIKE 1271.9 80%
379GLBR- 360 MATRIX SPIKE DUPLICATE 1590*8 99%
379GLBR- 384 * * 21NOV5:078SD10 965.4
379GLBR- 384 MATRIX SPIKE 2784.3 142%
379GLBR- 384 MATRIX SPIKE DUPLICATE 2824.7 143%
** = Mean of replicated sample.
U = Analyte detected below detection limits.
= Outside control limits.
Page 5
-------
BUFFALO RIVER PILOT PROJECT (CF#379)
OIL AND GREASE IN SEDIMENT SAMPLES
MSLCODE
SPQNSOR ID
OIL & GREASE
ug/g
REPLICATE ANALYSES
379GLBR- 111 Rep 1
379GLBR- 111 Rep 2
379GLBR- 111 Rep 3
379GLBR- 199 Rep 1
379GLBR- 199 Rep 2
379GLBR- 199 Rep 3
379GLBR- 269 Rep 1
379GLBR- 269 Rep 2
379GLBR- 269 Rep 3
379GLBR- 360 Rep 1
379GLBR- 360 Rep 2
379GLBR- 360 Rep 3
379GLBR- 384 Rep 1
379GLBR- 384 Rep 2
379GLBR- 384 Rep 3
22OCT5:563SA2O
22OCT5:563SA2O
22OCT5:563SA2O
30OCT4:013SB2O
30OCT4:013SB2O
30OCT4:013SB2O
1NOV10:157SB3O
1NOV10:157SB3O
1NOV10:157SB3O
20NOV3:278SC3O
20NOV3278SC3O
20NOV3:278SC30
21NOV5.078SD1O
21NOV5:078SD1O
21NOV5:078SD1O
U = Analyte detected below detection limits.
R = Reruns.
RSD% = Relative Standard Difference
= Outside control limits.
RSD %
RSD %
RSD %
RSD %
RSD %
2867.7
1839.4
2283.9
22% *
1634.5
1306.0
1610.2 R
12%
1436.9
1428.3
1633.9
8%
762.4
610.0 U
668.9 R
11%
974.5
748.9
1172.9
22% *
Page 6
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(ANALYZED 10/91)
5/22/92
(Concentrations in ng/g)
MSLCODE SPONSOR ID
379GLBR*15A 07OCT1:211SCO
379GLBRM5B 07OCT1211SCO
379GLBRM5C 07OCT1 21 1 SCO
379GLBR*17 07OCT1 2:091 SAO
379GLBR*21 07OCT12:531SBO
379GLBR*22 07OCT1 :521 SDO
Blank
STANDARD REFERENCE MATERIAL
SRM 1941
certified valut
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR*22 07OCT1 :521 SDO
379GLBR*22 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR*22 07OCT1 :521 SDO
379GLBR*22 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Naph- Acenaph- Acenaph-
thalene thylene thene Fluorene
47.16
38.15
35.59
37.64
34.39 U
147.09
16.79 U
831.66
NC
885.00
147.09
275.16
128.07
14% '
880.00
147.09
487.15
340.06
39% '
34.74 U
34.60 U
32.13 U
44.42 U
44.27 U
169.14
21.61 U
260.31 U
NC
885.00
169.14
319.31
150.17
17% *
880.00
169.14
714.45
545.31
62%
52.92
53.73
51.81
58.76 U
58.55 U
164.88
28.58 U
344.29 U
NC
885.00
164.88
297.06
132.18
15% '
880.00
164.88
678.57
513.69
58%
75.80
82.98
83.49
59.52
51.40 U
193.68
25.09 U
302.25 U
NC
885.00
193.68
325.32
131.64
15% *
880.00
193.68
773.71
580.03
66%
Phenan- Anthra-
threne cene
633.88
682.24
627.06
522.95
522.85
546.84
15.56 U
482.72
577.00
885.00
546.84
542.86
-3.98
0% *
880.00
546.84
1177.08
630.24
72%
157.45
178.79
159.06
110.44
118.72
246.40
18.44 U
222.14 U
202.00
885.00
246.40
371.73
125.33
14% *
880.00
246.40
921.38
674.98
77%
Fluoran-
thene
1160.98
1222.89
1106.10
1036.45
1398.88
1027.16
11.83U
1041.68
1220.00
885.00
1027.16
850.89
-176.27
-20% '
880.00
1027.16
1755.21
728.05
83%
Benzo(a)-
Pyrene Anthracene Chrysene
1017.31
1063.39
984.28
840.05
1137.65
859.27
12.24 U
988.04
N3
885.00
859.27
750.86
-108.41
-12%*
880.00
859.27
1565.81
706.54
80%
542.02
578.78
517.84
443.84
631 .32
561.82
10.57.U
486.81
550.00
885.00
561.82
583.86
22.04
2%'
880.00
561.82
1298.38
736.56
84%
675.73
691.00
649.86
581.27
756.99
665.26
9.36 U
630.54
NC
885.00
665.26
629.73
-35.53
-4% *
880.00
665.26
1332.46
667.2
76%
U > Detected below detection limit
' - Recoveries outside of QC limits.
NA - Not applicable.
NC - Not certified.
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(ANALYZED 10/91)
5/22/92
(Concentrations in ng/g)
MSLCODE
SPONSOR ID
Naph-
thalene
Acenaph-
thylene
Acenaph-
thene
Fluorene
Phenan-
threne
Anthra-
cene
Fluoran-
thene
Pyrene
Benzo(a)-
Anthracene
Chrysene
REPLICATE ANALYSIS
379GLBRM5A
379GLBRM5B
379GLBR*15C
07OCT1:211SCO
07OCT1:211SCO
070CT1:211SCO
RSD%
47.16
38.15
35.59
15%
34.74 U
34.60 U
32.13 U
NA
52.92
53.73
51.81
2%
75.80
82.98
83.49
5%
633.88
682.24
627.06
5%
157.45
178.79
159.06
7%
1160.98
1222.89
1106.10
5%
1017.31
1063.39
984.28
4%
542.02
578.78
517.84
6%
675.73
691.00
649.86
3%
U - Detected below detection limit
* - Recoveries outside of QC limits.
NA m Not applicable.
NC - Not certified.
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(ANALYZED 10/91)
5/22/92
MSLCODE
SPONSOR ID
(Concentrations
in ng/g)
Benzo(b)- Benzo(k)-
Fluoranthene Fluoranthene
Benzo(a)
Pyrene
lndeno(1,2
Pyrene
-3)
Dibenzo(a.h)
Anthracene
Benzo(g,h,i)
Perylene
% Surrogate Recovery
D8 Naph-
thalene
D10 Acenaph-
thaleneD12 Perylene
379GLBRM5A
379GLBRM5B
379GLBRM5C
379GLBRM7
379GLBR*21
379GLBR'22
Blank
07OCT1211SCO
07OCT1211SCO
07OCTV.211SCO
07OCT12:091 SAO
070CT12:531 SBO
07OCT1:521SDO
627.45
644.37
580.88
571.17
691.80
667.08
434.19
454.13
425.19
395.44
508.84
492.32
542.81
560.96
521.53
.477.87
584.10
554.67
438.57
453.05
426.39
408.35
491.21
560.12
103.80
114.59
106.08
94.88
116.89
331 .44
280.39
287.02
272.14
261.79
303.74
338.60
42%
36%*
34%*
49%
41%
55%
48%
50%
50%
57%
57%
62%
64%
67%
69%
72%
84%
77%
6.71 U
5.49 U
6.40 U
3.77 U
85%
85%
75%
STANDARD REFERENCE MATERIAL
SRM 1941
certified value
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR'22 07OCT1:521 SDO
379GLBR*22 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR*22 07OCT1:521SDO
379GLBR*22 -t Spike DUPLICATE
Amount Recovered
Percent Recovery
U - Detected below detection limit
* - Recoveries outside of QC limits.
NA » Not applicable.
NC - Not certified.
796.14
780.00
553.05
569.00
136.81
NC
423.60
516.00
69%
NA
74%
NA
82%
NA
885.00
667.08
629.73
-37.35
-4% '
880.00
667.08
1355.48
688.4
78%
885.00
492.32
510.06
17.74
2% *
880.00
492.32
1124.29
631.97
72%
885.00
554.67
549.35
-5.31
-1% *
880.00
554.67
1204.26
649.59
74%
885.00
560.12
507.53
-52.59
-6% '
880.00
560.12
1143.25
583.13
66%
885.00
331.44
450.56
119.12
13%'
880.00
331.44
1096.43
764.99
87%
885.00
338.60
375.92
37.32
4% *
880.00
338.60
837.02
498.42
57%
NA
55%
40%
NA
NA
NA
55%
52%
NA
NA
NA
62%
43%
NA
NA
NA
62%
70%
NA
NA
NA
77%
51%
NA
NA
NA
77%
93%
NA
NA
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379}
PAH ANALYSIS IN SEDIMENT SAMPLES
(ANALYZED 10/91)
5/22/92
MSLCODE
SPONSOR D
(Concentrations
in ng/g)
Benzo(b)- Benzo(k)-
Fluoranthene Fluoranthene
Benzo(a)
Pyrene
lndeno(1 ,2
Pyrene
.3)
Dibenzo(a.h)
Anthracene
Benzo(g,h,l)
Perylene
% Surrogate Recovery
D8 Naph-
thalene
010 Acenaph-
thaleneD12 Perylene
REPLICATE ANALYSIS
379GLBRM5A 07OCT1211 SCO 627.45 434.19 542.81 438.57 103.80 280.39 42%
379GLBR*15B 07OCT1211SCO 644.37 454.13 560.96 453.05 114.59 287.02 36%'
379GLBRM5C 07OCT1211SCO 580.88 425.19 521.53 426.39 106.08 272.14 34%'
RSD% 5% 3% 4% 3% 5% 3% NA
48%
50%
50%
NA
64%
67%
69%
NA
U » Detected below detection limit
* - Recoveries outside of QC limits.
NA - Not applicable.
NC - Not certified.
Page 4
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSLCode
379GLBR-97
379GLBR-97 -
379GLBR-128
379GLBR-132
379GLBR-160
379GLBR-161
379GLBR-164
379GLBR-204
379GLBR-187
379GLBR-226
379GLBR-227
379GLBR-252
379GLBR-253
379GLBR-256
379GLBR-257
379GLBR-286
379GLBR-326
379GLBR-331. Rep 1
379GLBR-331. Rep 2
379GLBR-331, Rep 3
379GLBR-361
379GLBR-366
379GLBR-370
Sponsor ID
I BIN A |
21OCT6:1810LA1O
21OCT62010LA1O
23OCT4:459LA2O
23OCT5:2010LA2O
25OCT10:1810LA3O
25OCT10:1910LA3O
25OCT9:549LA3O
30OCT4-.206LA3O
I BIN B I
25OCT3:0810LB1O
31OCT10:119LB2O
31 OCT1 0:231 OLB2O
31OCT3:119LB3O
31OCT3:109LB3O
31OCT3:0110LB30
31OCT3:0010LB3O
I BIN C |
18NOV5:559LC1O
19NOV5:509LC2O
19NOV5:0510LC20
19NOV5:0510LC2O
19NOV5:0510LC2O
20NOV2:193LC3O
20NOV2:429LC3O
20NOV3:0110LC30
Naph- Acenaph- Acenaph-
thalene thylene thene Flourene
134123
106763
39236
43851
24162
36540
38413
43 U
27983
10474
18845
13540
11561
14293
21054
18313
20689
5689
6110
5821
60 B
5181
9430
2361
2289
3069
4679
1751 #
3277 #
9204
46 U
5964
125 #
2714
202
155
2084
3789
2691
3444
1707
1504
1294
27 U
1358
5368
15805 #
14358
12181 *
9611 #
3970 #
7019 #
19760 #
62 U
7333 #
926 #
2273 #
2000 #
1896 #
2198#
4594 #
7161 *
9437 #
2801 #
2271 *
1920
36 U
1697
8325
37080 *
35122
32308
33598
12339
22862
64326
57 U
22981
2242
7796
6608
5939
5784
12089
23025
28310
7669
5291
4018
33 U
4305
18667
Phenan-
threne
86591 D
104808
110202
111982 0
55951 D
95140 0
189784 D
36 U
114021 D
6422
29804
32600 D
27611 D
29132 D
67219 D
83440 D
120301
44081
30611
23532
110
25498
91406 E
Anthra- Fluoran-
cene thene
15925
16862
18271
26274
11386
20580
39225
38 U
30532
239 #
6544
2759
1959
5948
14514
14407
22973
9728
6750
5246
23 U
7011
25842
8792
10929
16751
63737 D
37865 D
61455 D
35555
25 U
93778 D
1594
22030
14753 D
11711 D
18615 D
46912 D
17479
40218
33314
24642
19474
80
27038
81464 E
Page la
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSI Code
379GLBR-97
379GLBR-97 -
379GLBR-128
379GLBR-132
379GLBR-160
379GLBR-161
379GLBR-164
379GLBR-204
379GLBR-187
379GLBR-226
379GLBR-227
379GLBR-252
379GLBR-253
379GLBR-256
379GLBR-257
379GLBR-286
379GLBR-326
379GLBR-331, Rep 1
379GLBR-331, Rep 2
379GLBR-331. Rep 3
379GLBR-361
379GLBR-366
379GLBR-370
Sponsor ID
I BIN A
21OCT6:1810LA1O
21OCT65010LA1O
23OCT4-.459LA2O
23OCT5:2010LA2O
25OCT10:1810LA3O
25OCT10:1910LA3O
25OCT9:549LA3O
30OCT4:206LA3O
1 BINB
25OCT3:0810LB1O
31OCT10:119LB2O
31 OCT1 0:231 OLB2O
31OCT3:119LB3O
31OCT3:109LB3O
31OCT3:0110LB3O
31OCT3:0010LB3O
I BINC
18NOV5:559LC1O
19NOV5:509LC2O
19NOV5:0510LC2O
19NOV5:0510LC2O
19NOV5:0510LC2O
20NOV2-.193LC3O
20NOV2:429LC3O
20NOV3:0110LC3O
Benzo[a]- Benzo(b)- Benzo(k)- Benzo(a)- [1,
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
33900 D
39571
49386
64875 0
37935 D
62018 D
94035 D
26 U
71800 D
2328
15136
13079 D
10912 D
13914 D
35469 D
39512 D
63531
28145
20062
15593
68
21804
62530 E
11082
11015
17602
24528
12637
19820
38129
30 U
18980
603
5037
3456
2989
4293
11296
14062
23436
7718
5570
4340
18 U
6941
17229
33172 D
40731
39751
50826
28396 0
45983 D
77380 D
25 U
.A
30291 D
1561
7478
6596
5688
6558
17116
30385 D
46161
13840
9516
7121
31
10309
24776
8935
9968
10321
32041
31 U
38
32084
24 U
32 U
611
6273
3147
2684
3304
8869
10454
18852
6160
4514
3824
17#
9689
14282
21 U
84 U
153U
51 U
10940
17677
37 U
17U
14581
24 U
24 U
9 U
8
1580*
21 U
22 U
96 U
2558
2063
1461
10U
69 U
5931 #
13481 #
13156
11148
16437
8325
13742
28968
24 U
7690
212 *
1585
1020
972
1466
3867
8401
13019
3801
2425
1911
14 U
2958
6370
Indeno
2,3-cd]-
pyrene
1451
1169
1104
. 4268
2174
3389
5098
22 U
2579
80
614
266
225
596
1517
1369
2202
1260
925
716
13 U
1128
3062
Page Ib
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSI Code
379GLBR-97
379GLBR-97 *
379GLBR-128
379GLBR-132
379GLBR-160
379GLBR-161
379GLBR-164
379GLBR-204
379GLBR-187
379GLBR-226
379GLBR-227
379GLBR-252
379GLBR-253
379GLBR-256
379GLBR-257
379GLBR-286
379GLBR-326
379GLBR-331. Rep 1
379GLBR-331. Rep 2
379GLBR-331. Rep 3
379GLBR-361
379GLBR-366
379GLBR-370
Dibenzo(a.h)-
Sponsor ID anthracene
I BIN A
21OCT6:1810LA1O
21OCT6:2010LA1O
23OCT4:459LA2O
23OCT5:2010LA2O
25OCT10:1810LA3O
25OCT10:1910LA3O
25OCT9:549LA3O
30OCT4:206LA3O
I BINB
25OCT3:0810LB1O
31OCT10:119LB2O
31 OCT1 0:231 OLB2O
31OCT3:119LB3O
31OCT3:109LB3O
31OCT3:0110LB3O
31OCT3:0010LB3O
I BINC
18NOV5:559LC1O
19NOV5-.509LC2O
19NOV5:0510LC2O
19NOV5:0510LC2O
19NOV5:0510LC2O
20NOV2:193LC3O
20NOV2:429LC3O
20NOV3:0110LC3O
I
3323*
3229
2086*
3406*
1960*
3413*
5963*
21 U
I
1616*
68*
211
188*
190*
213
543
I
1702*
2373*
688*
428*
261 #
12U
426
997
Benzo[ghi]
perylene
6622
7315
7981
7772
4423
7099
16790
27 #
3648
208
602
523
528
610
1525
5736
8312
1873
1223
882
11 B
1278
3062
% Surrogate Recovery
D8-
Naphthalene
23% *
20%*
12% *
16%*
43%
41%
9% *
82%
68%
16% *
24% *
24% *
22% *
21% *
21% *
16% *
12% *
20% '
27% *
24% *
28% '
18% *
21% *
D-10 Ace-
naphthalene
31% *
29%'
22% *
21% *
53%
50%
28% *
81%
61%
24%*
31% *
33% *
32% *
30% *
28% *
31% *
22%*
29% *
33% *
33% *
31% *
30% *
31% *
D12-
Perylene
27%*
33% *
23%*
24% *
55%
48%
34%*
83%
66%
23%*
31%'
29% *
30% *
32%'
28%*
33%*
27%'
36% *
37%*
34% *
38% *
29%*
32%*
Page Ic
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSLCode
379GLBR-398
379GLBR-404
379GLBR-275
BLANK
Sponsor ID
I BIN D |
21NOV3:2610LD1O
21NOV4:169LD1O
I DILUTION WATER I
6NOV12:003LO
Naph- Acenaph- Acenaph-
thalene thylene thene
5543
4211
30 B
85
819
2106
19U
53 U
1796 *
2095*
26 U
70 U
Flourene
4039
7287
24 U
65 U
Phenan-
threne
19280
36954
34
41 U
Anthra-
cene
3992
11917
16 U
44 U
Fluoran-
thene
15163
39774
32
29 U
MATRIX SPIKE RESULTS (1)
Amount Spiked
379GLBR-132
379GLBR-132 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-132
379GLBR-132 + Spike
Amount Recovered
Percent Recovery
23OCT5:2010LA2O
23OCT5:2010LA2O
DUPLICATE
6410
43851
23639
-20212
•315%*
7143
43851
48960
5109
72%
6410
4679
3869
-810
-13%*
7143
4679
6735
2056
29% *
6410
9611 #
6324 #
-3287
-51%*
7143
9611 *
11133
1522
21% *
6410
33598
20300
-13298
-207% *
7143
33598
34056
458
6% *
6410
111982 D
68000
-43982
-686% *
7143
111982 D
126052 E
14070
1 97% *
6410
26274
16648
-9626
-150%'
7143
26274
28647
2373
33% *
6410
63737 D
39157
-24580
-383% *
7143
63737 D
71703
7966
112%
Page 2a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSI Code Sponsor ID
I BIND
379GLBR-398 21NOV3:2610LD10
379GLBR-404 21NOV4:169LD1O
I DILUTION WATER
379GLB R-275 6NOV12:003LO
BLANK
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-132 23OCT5:2010LA2O
379GLBR-132 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-132 23OCT5:2010LA2O
379GLBR-132 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Benzo[a]-
Pyrene anthracene
12281 3051
30273 9684
65 13 U
30 U 34 U
6410 6410
64875 D 24528
40044 154397
-24831 129869
-387% * 2026% *
7143 7143
64875 D 24528
71305 25861
6430 1333
90% 19% *
Benzo(b)- Benzo(k)- Benzo[a]- [1
Chrysene Fluoranthene Fluoranthene pyrene
5001
14186
19
29 U
6410
50826
30532
-20294
-317%*
7143
50826
53761
2935
41%
4089
7395
10 U
27 U
6410
32041
13969
-18072
-282% *
7143
32041
23306
-8735
-122% *
57
3751
7 U
20 U
6410
51 U
5378
5378
84%
7143
51 U
10431
10431
146% *
1097
3365
10 U
27 U
6410
16437
10568
-5869
-92% *
7143
16437
16661
224
3% *
Indeno
2.3-cd]-
pyrene
537
1217
. 9 U
25U
6410
4268
3727
-541
-8% *
7143
4268
6394
2126
30% *
Page 2b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSLCode
1
379GLBR-398
379GLBR-404
1
379GLBR-275
BLANK
Sponsor ID
BIND
21NOV3:2610LD1O
21NOV4:169LD1O
DILUTION WATER
6NOV12:003LO
Dibenzo[a,h]-
anthracene
I
210
386
I
9 U
24 U
Benzo[ghi]
perylene
521
1201
10 B
33
% Surrogate Recovery
D8-
Naphthalene
26% *
8%*
21%*
61%
D-10 Ace-
naphthalene
29%*
15%*
28% *
64%
012-
Perylene
24%
13%
38%
67%
MATRIX SPIKE RESULTS
Amount Spiked
379GLBR-132
379GLBR-132 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-132
379GLBR-132 + Spike
Amount Recovered
Percent Recovery
23OCT5:2010LA2O
23OCT5:2010LA2O
DUPLICATE
6410
3406 #
3654
248
4%*
7143
3406 #
5462
2056
29% *
6410
7772
5550
-2222
-35% '
7143
7772
9791
2019
28% *
NA
16% *
14% *
NA
NA
NA
16% *
18% *
NA
NA
NA
21%*
21%*
NA
NA
NA
21%*
23% *
NA
NA
NA
24%
24%
NA
NA
NA
24%
25%
NA
NA
Page 2c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
MSLCode
Sponsor ID
Naph-
thalene
Acenaph-
thylene
Acenaph-
thene
Flourene
Phenan-
threne
Anthra-
cene
Fluoran-
thene
REPLICATE ANALYSIS
379GLBR-331. Rep 1 19NOV5:0510LC2O 5689 1707 2801 # 7669 44081 9728 33314
379GLBR-331. Rep 2 19NOV5:0510LC2O 6110 1504 2271 # 5291 30611 6750 24642
379GLBR-331, Rep 3 19NOV5:0510LC20 5821 1294 1920 4018 23532 5246 19474
RSD% 4% 14% 19% 33% * * 32% * • 32% * * 27% * *
Page 3a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSLCode
Sponsor
ID
Pyrane
Benzo(a]-
anthracene
Chrysene
Benzo(b)-
Fluoranthene
Benzo(k)-
Fluoranthene
Indeno
Benzo(a)- [1,2.3-cd]-
pyrene
pyrene
REPLICATE ANALYSIS
379GLBR-331. Rep 1
379GLBR-331, Rep 2
379GLBR-331. Rep 3
19NOV5:OS10LC2O
19NOV5:0510LC2O
19NOV5-.0510LC2O
RSD%
28145
20062
15593
30% *
7718
5570
4340
29%
13840
9516
7121
34% * *
6160
4514
3824
25%
2558
2063
1461
27% * *
3801
2425
1911
36%
1260
925
716
28%
Page 3b
-------
BUFFALO RIVER PILOT PROJECT (*379)
PAH ANALYSIS IN WATER SAMPLES
(Concentrations in ng/L)
MSLCode
Sponsor ID
Dibenzo[a,h]-
anthracene
Benzo[ghi]
perylene
% Surrogate Recovery
Da-
Naphthalene
D-10 Ace-
naphthalene
D12-
Perylene
REPLICATE ANALYSIS
379GLBR-331. Rep 1
379GLBR-331, Rep 2
379GLBR-331. Rep 3
19NOV5:0510LC2O 688 #
19NOV5:0510LC2O 428 #
19NOV5:0510LC2O 261 #
RSD% 47% *
1873
1223
882
38% * *
20%
27%
24%
NA
29%
33%
33%
NA
36%
37%
34%
NA
U - Detected at or below detection limit.
B • Naphthalene and Benzo(ghi)perylene were detected at levels near detection limits.
- • Field replicate.
* m Indicates confirming ion out of specification.
D • 10:1 sample dilution.
E » Indicates value outside of calibration.
RSD % • Relative standard deviation.
* - Recoveries exceed laboratory control limits (40-120%).
" m Value exceeds precision goal of 20%.
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-13
379GLBR-16
379GLBR-57
379GLBR-58
379GLBR-59
379GLBR-104
379GLBR-107
379GLBR-108
379GLBR-111
379GLBR-111-R
379GLBR-113
379GLBR-122
379GLBR-122-R
379GLBR-123
379GLBR-124
379GLBR-124-R
379GLBR-136
379GLBR-139
379GLBR-141
379GLBR-143
379GLBR-145
379GLBR-151
379GLBR-152
379GLBR-153
379GLBR-166
379GLBR-167
Naph- Acenaph- Acenaph- Dibenzo-
Sponsor ID thalene thylene thene Flourena thiophene
I BIN A |
07OCT1 2:341 SAO
07OCT2:401SAO
09OCT11:502SA30
09OCT11:382SA20
09OCT11:282SA10
22OCT11:317SA10
22OCT11:378SA10
22OCT4-.203SA2O
22OCT5-.563SA2O
22OCT5-.563SA2O
23OCT1:303SA2O
23OCT4-.284SA2O
23OCT4:284SA2O
23OCT4:274SA2O
23OCT4:294SA2O
23OCT4:294SA2O
24OCT10:457SA20
24OCT10:508SA2O
24OCT2:203SA3O
24OCT5:503SA3O
24OCT6:203SA3O
25OCT9:224SA3O
25OCT9:224SA3O
250CT9-.214SA30
25OCT9-.307SA30
25OCT9:368SA3O
73
62
102
66
67
573
126
35
158
36 U
65
24
45
39
47
61
221
275
23 U
44
60
25
27
9
36
33
34
34
42
46
31
29
16
35
88
44
33
4 U
5 U
7 U
4 U
6 U
13
14U
49
34
29
6 U
8 U
7 U
14
8 U
35
36
52
93
39
162 *
25 #
43
109
53 U
40
7 U
8 U
13 U
7 U
11 U
70
31 #
38
45
46
10 U
14 U
12U
18
15U
64
64
80
138
69
560
102
81
160
46
59
5 U
6 U
10 U
6
7 U
198
97
56
62
67
7 U
12
10 U
48
18
34
43
42
67
39
1884
167
44
82
32
38
4 U
15
9
8
21
476
218
36
41
39
9
15
11
72
28
Phenan-
threne
437
475
552
948
473
2716
593
608
1166
446
462
21
38
29
34
64
832
405
543
605
453
101
180
109
540
187
Anthra-
cene
96
95
120
180
104
373
141
118
230
93
91
4 U
4 U
6 U
4 U
7
137
65
85
82
80
17
24
17
110
38
Fluoran-
thene
1101
1160
1363
1731
1169
. 2271
1448
1326
2726
978
1114
14
20
21
26
59
566
250
1162
1308
1060
198
400
263
1890
584
Page la
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-13
379GLBR-16
379GLBR-57
379GLBR-58
379GLBR-59
379GLBR-104
379GLBR-107
379GLBR-108
379GLBR-111
379GLBR-111-R
379GLBR-113
379GLBR-122
379GLBR-122-R
379GLBR-123
379GLBR-124
379GLBR-124-R
379GLBR-136
379GLBR-139
379GLBR-141
379GLBR-143
379GLBR-145
379GLBR-151
379GLBR-152
379GLBR-153
379GLBR-166
379GLBR-167
Sponsor ID
I BIN A |
07OCT1 2:341 SAO
07OCT2:401SAO
09OCT11:502SA3O
09OCT11:382SA2O
09OCT1V.282SA1O
22OCT11:317SA1O
22OCT11-.378SA1O
22OCT4:203SA2O
22OCT5:563SA2O
22OCT5:563SA2O
23OCT1:303SA2O
23OCT4:284SA2O
23OCT4:284SA2O
23OCT4-.274SA2O
23OCT4:294SA2O
23OCT4:294SA20
24OCT10:457SA20
24OCT10:508SA20
24OCT2:203SA3O
24OCT5:503SA3O
24OCT6:203SA3O
25OCT9:224SA3O
25OCT9-.224SA3O
25OCT9:214SA3O
25OCT9:307SA3O
25OCT9:368SA3O
Benzo[a]- Benzo(b)- Benzo(k)- Benzofa]- [1,
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
792
827
962
1220
845
3071
1114
937
1863
737
805
6
18
15
19
46
620
246
788
906
777
136
248
173
1273
380
409
394
483
638
410
1933
888
489
918
339
433
3 U
8
9
10
21
381
139
360
429
367
73
148
104
812
350
553
583
659
767
569
3326
1277
609
1335
487
585
8
17
15
21
41
610
263
589
703
521
124
267
166
1155
536
612
677
790
987
663
2920
1740 #
772
1528
507
680
4
19
11 #
19
52
744
361
676
828
629
200
326
206
1289 #
783
485
479
521
658
458
4 U
930 #
537
1022
373
476
2 U
2 U
5 #
2 U
3 U
340*
8 U
496
611
477
2 U
218
135
747 #
424
497
501
519
634
471
1821
972
503
845
372
447
3 U
4
4 U
3 U
10
337
119
368
408
459
46
96
95
614
306
Indeno
2.3-cd]-
pyrene
370
391
449
545
376
6.57
749
433
816
294
372
2 U
3
3
2
7
302
71
369
443
362
33
151
90
428
240
Page Ib
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code
379GLBR-13
379GLBR-16
379GLBR-57
379GLBR-S8
379GLBR-59
379GLBR-104
379GLBR-107
379GLBR-108
379GLBR-111
379GLBR-111-R
379GLBR-113
379GLBR-122
379GLBR-122-R
379GLBR-123
379GLBR-124
379GLBR-124-R
379GLBR-136
379GLBR-139
379GLBR-141
379GLBR-143
379GLBR-145
379GLBR-151
379GLBR-152
379GLBR-153
379GLBR-166
379GLBR-167
Sponsor ID
I BIN A
07OCT1 2:341 SAO
07OCT2:401SAO
09OCT11:502SA3O
09OCT11:382SA2O
09OCT11:282SA1O
22OCT11:317SA1O
22OCT11:378SA1O
22OCT4:203SA2O
22OCT5:563SA2O
22OCT5:563SA2O
23OCT1:303SA2O
23OCT4:284SA2O
23OCT4:284SA2O
23OCT4-.274SA2O
23OCT4:294SA2O
23OCT4:294SA2O
24OCT10:457SA2O
24OCT10:508SA2O
24OCT2:203SA3O
24OCT5:503SA3O
24OCT6:203SA3O
25OCT9:224SA3O
25OCT9:224SA3O
25OCT9:214SA3O
25OCT9:307SA3O
25OCT9.-368SA3O
Dibenzo[a,h]-
anthracene
I
141
150
182
200
151
501 »
335
124
330
74
150
3 U
2
3 U
3 U
4
140
42
123
163
97
17
67
44
162
96
Benzo(ghi)
perylene
358
368
397
480
316
1269
798
385
582
294
364
2 U
3
4
5
7
314
89
345
399
363
30
135
85
441
239
d8 Naph-
thalene
77%
62%
90%
81%
54%
52%
64%
39% *
42%
33% *
43%
24% *
67%
68%
39% *
71%
50%
80%
4% *
53%
98%
74%
67%
17% *
59%
61%
% Surrogate
Recovery
d10 Acena- 010-
phthene Fluorene
73%
66%
72%
48%
54%
25% *
34% *
26% *
36% *
72%
41%
9% *
73%
35% *
26% *
80%
45%
71%
48%
50%
89%
80%
54%
54%
68%
62%
99%
96%
103%
97%
86%
88%
87%
79%
75%
65%
75%
52%
75%
80%
63%
73%
74%
83%
69%
82%
97%
77%
81%
72%
78%
79%
D14 Oibenzo-
(a.h)Anthracene
131%
132%
129%
111%
116%
97%
102%
94%
89%
91%
93%
4%
21%
15%
25%
34%
85%
82%
96%
110%
111%
41%
90%
76%
99%
88%
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-14
379GLBR-23
379GLBR-65
379GLBR-66
379GLBR-67
379GLBR-174
379GLBR-176
379GLBR-181
379GLBR-182. Rep 1
379GLBR-182. Rep 2
379GLBR-182. Rep 3
379GLBR-183
379GLBR-193
379GLBR-196
379GLBR-198
379GLBR-199, Rep 1
379GLBR-199. Rep 2
379GLBR-199, Rep 3
379GLBR-206
379GLBR-210
379GLBR-213
379GLBR-220
379GLBR-220-R
379GLBR-221
379GLBR-221-R
379GLBR-222
379GLBR-222-R
379GLBR-242
379GLBR-243
379GLBR-244
379GLBR-247
Sponsor ID
I BINB
07OCT1:101SBO
07OCT1:011SBO
09OCT9:542SB1O
Naph- Acenaph- Acenaph- Dibenzo- Phenan- Anthra-
thalene thylene thene Flourene thiophene throne cene
79
109
53
09OCT10:152SB2O 135
09OCT10:352SB3O 1 1 5
25OCT12:153SB1O 76
25OCT2:153SB1O
25OCT2:254SB1O
25OCT2:294SB1O
25OCT2:294SB1O
25OCT2294SB1O
25OCT2.-284SB1O
25OCT3:527S81O
25OCT3:578SB1O
30OCT2:493SB2O
20OCT3:573SB2O
20OCT3:573SB2O
20OCT3:573SB2O
30OCT4:413SB2O
31OCT9:027SB2O
31OCT9:078SB20
31OCT9:264SB2O
31OCT9:264SB2O
31OCT9:254SB2O
31OCT9:254SB2O
31OCT9:244SB2O
31OCT9:244SB2O
40
23
27
22
26
20
65
50
44
62
49
59
63
375
161
19
30
18
28
24 U
44
31OCT10:453SB3O 35
31OCT11:503SB3O 60
31OCT2:303SB3O
31OCT2:384SB3O
47
21
57
46
33
38
37
32
32
8
7 U
11 U
11 U
10U
17
18
32
31
29
23
43
24
8 U
17U
6 U
10U
4 U
20U
9 U
29
34
32
12 U
34
41
55
62
64
49
49
10U
12U
69 #
72 #
58 *
30 #
28
59 #
52
42
40
268*
46 #
15U
28 U
11 U
16 U
8 U
36 U
15 U
49
36
103 #
22 #
64
87
87
91
79
68
74
27
16
21
16
12U
111
101
105
74
59
61
222
142
42
22 U
8 U
13 U
6 U
SOU
11 U
56
56
70
14 U
38
49
55
56
46
42
47
144
11
18
14
10
116
88
55
48
40
44
127
142
53
14U
6 U
8 U
5 U
20 U
8 U
39
37
49
16
425
593
550
640
562
425
564
338
146
191
143
115
887
942
727
503
424
472
2131
750
287
12 U
19
10
15
17 U
19
499
426
614
90
108
123
117
148 .
125
81
106
38
18
35
29
19
191
203
152
91
81
93
429
146
47
14 U
5 U
8 U
4 U
19U
7 U
96
87
128
13
Fluoran-
thene
1182
1447
1172
1536
1379
957
'1245
418
274
356
277
209
2301 D
2599 0
1239
1123
931
892
2920
1173
420
10 U
7
6 U
4
17U
6 U
1005
1032
1197
166
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-14
379GLBR-23
379GLBR-65
379GLBR-66
379GLBR-67
379GLBR-174
379GLBR-176
379GLBR-181
379GLBR-182. Rep 1
379GLBR-182, Rep 2
379GLBR-182. Rep 3
379GLBR-183
379GLBR-193
379GLBR-196
379GLBR-198
379GLBR-199, Rep 1
379GLBR-199. Rep 2
379GLBR-199, Rep 3
379GLBR-206
379GLBR-210
379GLBR-213
379GLBR-220
379GLBR-220-R
379GLBR-221
379GLBR-221-R
379GLBR-222
379GLBR-222-R
379GLBR-242
379GLBR-243
379GLBR-244
379GLBR-247
Sponsor ID
I BIN B |
07OCT1:101SBO
07OCT1:011SBO
09OCT9:542SB1O
09OCT10:152SB2O
09OCT10:352SB3O
25OCT12:153SB1O
25OCT2:153SB1O
25G<;T2:254SB1O
25OCT2:294SB1O
25OCT2:294SB1O
25OCT2:294SB1O
25OCT2:284SB1O
25OCT3-.527SB1O
25OCT3:578SB1O
30OCT2:493SB2O
20OCT3:573SB2O
20OCT3:573SB2O
20OCT3-.573SB2O
30OCT4:413SB2O
31OCT9:027SB2O
31OCT9:078SB2O
31OCT9:264SB2O
31OCT9:264SB2O
31OCT9:254SB2O
31OCT9:254SB2O
31OCT9:244SB2O
31OCT9:244SB2O
31OCT10-.453SB3O
31OCT11:503SB3O
31OCT2:303SB3O
31OCT2:384SB3O
Indeno
Benzo[a]- Benzo(b)- Benzo(k)- Benzo[aJ- [1,2.3-cdJ-
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene pyrene
887
1021
868
1128
999
720
872
409
173
254
196
139
1616D
1848
933
833
696
649
2310
775
258
9 U
7
5 U
4
15U
5 U
761
757
905
109
455
491
451
571
520
347
561
209
98
145
122
87
1162
1001
472
376
322
298
1197
620
230
8 U
4 U
5 U
3 U
14 U
5 U
359
373
463
73
630
695
583
742
695
480
959
371
187
217
195
151
1584 D
1354
614
517
433
410
1371
863
369
7 U
5
4 U
3
13 U
5 U
508
500
603
132
789
797
723
874
791
596
859
349
243
239
231
176
1873
1386 #
683
631
499
470
1364
1340
501
7 U
4 U
4 U
3 U
15U
5 U
580
605
695
253
546
540
511
581
558
416
622
189 *
147
154
137
111
969*
858*
515
457
378
335
1075
738
206*
6 U
3 U
4 U
2 U
13U
4 U
441
441
482
4 U
654
564
519
655
585
453
397
196
29
97
94
58
836
638
510
447
383
343
1058
615
113
8 U
3 U
5 U
3 U
16 U
5 U
434
423
512
53
544
444
413
483
452
337
418
168
104
107
100
86
538
433
395
355
295
268
771
613
83
5 U
2 U
3 U
2 U
10U
4 U
340
347
378
67
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSLCode
379GLBR-14
379GLBR-23
379GLBR-65
379GLBR-66
379GLBR-67
379GLBR-174
379GLBR-176
379GLBR-181
379GLBR-182, Rep 1
379GLBR-182. Rap 2
379GLBR-182, Rep 3
379GLBR-183
379GLBR-193
379GLBR-196
379GLBR-198
379GLBR-199. Rep 1
379GLBR-199, Rep 2
379GLBR-199, Rep 3
379GLBR-206
379GLBR-210
379GLBR-213
379GLBR-220
379GLBR-220-R
379GLBR-221
379GLBR-221-R
379GLBR-222
379GLBR-222-R
379GLBR-242
379GLBR-243
379GLBR-244
379GLBR-247
Sponsor ID
I BINB
07OCT1:101SBO
07OCT1:011SBO
09OCT9:542SB1O
09OCT10:152SB2O
09OCT10:352SB3O
25OCT12:153SB1O
25OCT2:153SB1O
25OCT2-.254SB1O
25OCT2:294SB1O
25OCT2294SB1O
25OCT2:294SB1O
25OCT2:284SB1O
25OCT3:527SB1O
25OCT3:578SB1O
30OCT2:493SB2O
20OCT3:573SB2O
20OCT3:573SB2O
20OCT3:573SB20
30OCT4:413SB20
31GOT9:027SB2O
31OCT9:078SB2O
31OCT9:264SB20
31OCT9:264SB2O
31OCT9-.254SB2O
31OCT9:254SB20
31OCT9:244SB2O
31OCT9:244SB2O
31OCT10:453SB3O
31OCT11:503SB3O
31OCT2:303SB3O
31OCT2:384SB3O
Dibenro[a.hJ-
anthracene
I
307
171
161
195
182
118
161
73
48
51
48
40
231
178
113
130
106
96
311
255
53
6
3
3
2
12
4
92
129
109
32
Benzo(ghi]
perylene
642
401
366
422
388
340
383
189
90
99
96
86
569
444
379
353
291
253
709
618
67
U 5 U
U 3 U
U 3 U
U 2 U
U 11 U
U 4 U
326
324
374
64
d8 Naph-
thalene
75%
91%
66%
83%
84%
78%
54%
52%
62%
47%
66%
47%
66%
69%
46%
87%
74%
70%
54%
87%
80%
47%
63%
45%
73%
10% *
77%
40%
74%
49%
50%
% Surrogate
Recovery
d10 Acena- 010-
phthene Fluorene
69%
78%
45%
64%
64%
65%
54%
65%
45%
43%
62%
43%
58%
56%
51%
73%
62%
61%
50%
76%
65%
23% *
66%
39% *
74%
40%
80%
39% *
64%
48%
39% *
90%
109%
90%
107%
100%
79%
79%
78%
78%
64%
78%
63%
85%
80%
72%
94%
78%
78%
75%
96%
88%
60%
65%
57%
77%
71%
75%
66%
85%
71%
55%
D14 Dibanzo-
(a.h)Anthracene
122%
145%
104%
132%
123%
86%
102%
93%
89%
73%
87%
73%
101%
93%
91%
105%
87%
89%
95%
117%
55%
5%
3%
7%
3%
5%
5%
86%
101%
92%
63°/c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-247-R
379GLBR-248
379GLBR-249
379GLBR-268
379GLBR-268-R
379GLBR-269
379GLBR-18. Rep 1
379GLBR-18, Rep 2
379GLBR-18, Rep 3
379GLBR-20
379GLBR-73
379GLBR-74
379GLBR-75
379GLBR-280
379GLBR-282
379GLBR-284
379GLBR-288
379GLBR-302
379GLBR-303
379GLBR-304
379GLBR-307
379GLBR-311
379GLBR-313
379GLBR-315
379GLBR-323, Rep 1
379GLBR-323. Rep 2
379GLBR-323, Rep 3
379GLBR-324
Naph- Acenaph- Acenaph- Dibenzo-
Sponsor ID thalene thylene thene Flourene thiophene
I BIN B |
31OCT2:384SB3O
31OCT2:354SB3O
31OCT2:364SB3O
1NOV10:208SB3O
1NOV10:208SB3O
1NOV10:157SB30
I BIN C |
07OCTV331SCO
07OCT1331SCO
07OCTV.331SCO
07OCTV.441SCO
09OCT4:562SC1O
09OCT4:352SC20
09OCT4:162SC3O
18NOV2:553SC1O
18NOV3:503SC1O
18NOV4:403SC1O
18NOV6:1510LC10
19NOV8:594SC1O
19NOV9:004SC1O
19NOV9:014SC10
19NOV9238SC1O
19NOV11:303SC20
19NOV2203SC2O
19NOV3:553SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
45 U
21
26
81
109
84
147
94
125
105
101
94
121
67
68
113
115
33
23
27
281
109
78
34
36
31
31
34
39 U
7 U
15U
8 U
20 U
14
66
41
53
34
53
41
43
44
32
60
41
7 U
11 U
11 U
13
39
48
29
7 U
10
7 U
12 U
68 U
13 U
26 U
15 U
36 U
22
92
67
91
59
97
78
69
65*
72
134
57
13 U
18 U
21 *
41 #
81
87
54
12U
10 U
11 U
21 U
9 U
10U
19 U
34
38
61
147
95
131
101
153
105
105
91
108
173
128
11 U
13U
13U
121
118
111
85
10U
13
9 U
17 U
21
18
16
74
76
137
105
75
100
77
105
78
73
69
79
134
216
16
22
19
304
87
88
67
24
28
22
56
Phenan-
threne
141
101
96
364
450
612
923
615
835
570
875
661
659
613
697
1155
1197
98
125
98
799
684
713
550
128
174
125
142
Anthra-
cene
18
11
13
60
85
107
264
167
237
143
193
164
151
130
136
244
277
15
22
16
104
144
153
133
20
28
20
19
Fluoran-
thene
171
191
196
763
771
. 1253
1938
1343
1793
1245
1552
1397
1444
1139
1328
1975
4360
212
286
211
1069
1334 D
1295
1080
267
379
265
229
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code
379GLBR-247-R
379GLBR-248
379GLBR-249
379GLBR-268
379GLBR-268-R
379GLBR-269
379GLBR-18. Rep 1
379GLBR-18, Rep 2
379GLBR-18, flap 3
379GLBR-20
379GLBR-73
379GLBR-74
379GLBR-75
379GLBR-280
379GLBR-282
379GLBR-284
379GLBR-288
379GLBR-302
379GLBR-303
379GLBR-304
379GLBR-307
379GLBR-311
379GLBR-313
379GLBR-315
379GLBR-323, Rep 1
379GLBR-323. Rep 2
379GLBR-323, Rep 3
379GLBR-324
Sponsor ID
I BIN B |
31OCT2:384SB3O
31OCT2:354SB3O
31OCT2:364SB3O
1NOV10:208SB3O
1NOV10:208SB3O
1NOV10:157SB3O
I BIN C |
07OCT1:331SCO
07OCT1331SCO
07OCTV331SCO
O7OCTIL441SCO
09OCT41S62SC1O
09OCT4t352SC20
09OCT4:162SC3O
18NOV2:553SC1O
18NOV3:503SC1O
18NOV4:403SC1O
18NOV6:1510LC10
19NOV8:594SC1O
19NOV9:004SC1O
19NOV9:014SC1O
19NOV9238SC1O
19NOV11:303SC20
19NOV2203SC2O
19NOV3:553SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
Benzo[a]-
Pyrene anthracene
121
116
129
475
507
822
1534
1077
1436
972
1211
1073
1098
939
1022
1597
3446
145
205
152
963
1057 D
1058
843
189
277
180
156
87
70
89
360
391
700
785
528
747
477
615
533
541
467
470
782
1879
101
157
114
633
473
494
407
131
178
126
113
Benzo(b)- Benzo(k)- Benzo(a)- [1
Chrysene Fluoranthene Fluoranthene pyrene
156
131
160
562
637
1031
957
664
893
634
762
692
704
634
601
999
2446
184
264
199
1175
655
682
526
238
296
240
209
262
163
175
806
1217
1639
1039
766
1033
700
921
761
794
696
715
1054
4861
383
322
245
1566
764
755
618
484
361
308
245
3 U
97
106
422*
8 U
904*
777
513
695
475
634
537
560
537
503
826
10 U
4 U
204
140
4 U
542
539
424
4 U
229
174
145
60
43
59
281
286
719
912
601
852
522
639
598
608
577
556
872
1664*
97
148
102
605
622
590
465
131
189
123
82
Indeno
,2.3-cd]-
pyrene
59
62
70
249
254
595
621
438
583
385
515
436
457
407
396
614
1095
105
164
117
302
414
413
337
137
180
141
125
Page 3b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code
379GLBR-247-R
379GLBR-248
379GLBR-249
379GLBR-268
379GLBR-268-R
379GLBR-269
379GLBR-18. Rep 1
379GLBR-18, Rep 2
379GLBR-18. Rep 3
379GLBR-20
379GLBR-73
379GLBR-74
379GLBR-75
379GLBR-280
379GLBR-282
379GLBR-284
379GLBR-288
379GLBR-302
379GLBR-303
379GLBR-304
379GLBR-307
379GLBR-31 1
379GLBR-313
379GLBR-315
379GLBR-323, Rep 1
379GLBR-323. Rep 2
379GLBR-323, Rep 3
379GLBR-324
Dibenzo[a,hJ- Benzo[ghi]
Sponsor ID anthracene perylene
I BINB
31OCT2:384SB3O
31OCT2:354SB3O
31OCT2:364SB30
1NOV10:208SB30
1NOV10:208SB30
1NOV10:157SB3O
I BINC
07OCT1331SCO
07OCT1331SCO
07OCT1:331SCO
07OCT1:441SCO
09OCT4-.562SC1O
09OCT4-.352SC20
09OCT4:162SC3O
18NOV2:553SC1O
18NOV3:503SC10
18NOV4:403SC1O
18NOV6:1510LC10
19NOV8:594SC10
19NOV9:004SC10
19NOV9:014SC1O
19NOV9238SC1O
19NOV11:303SC2O
19NOV2203SC2O
19NOV3-.553SC2O
19NOV4-.504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
30 62
31 54
35 65
108 224
116 261
249 571
251 602
179 388
241 505
161 345
195 475
176 397
183 415
150 394
156 368
236 585
481 1154
48 104
76 165
52 117
170 456
159 407
152 397
117 336
54 144
71 189
55 146
55 128
d8 Naph-
thalene
1% *
55%
61%
61%
76%
70%
64%
57%
72%
80%
84%
78%
87%
59%
54%
65%
69%
90%
62%
54%
58%
96%
65%
37% *
86%
84%
83%
52%
% Surrogate
Recovery
d10 Acena- 010-
phthene Fluorene
131% *
59%
41%
31% *
82%
65%
59%
61%
68%
69%
46%
76%
61%
48%
61%
30% *
63%
80%
43%
32% *
70%
89%
54%
46%
77%
76%
74%
48%
52%
82%
74%
71%
78%
91%
89%
84%
96%
100%
104%
101%
102%
79%
91%
87%
85%
99%
79%
71%
82%
111%
85%
80%
89%
91%
88%
74%
014 Dibenzo-
(a.h)Anthracene
67%
79%
74%
64%
78%
111%
123%
121%
133%
133%
116%
129%
122%
93%
106%
89%
124%
104%
91%
78%
100%
130%
97%
101%
96%
101%
99%
87%
Page 3c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code
379GLBR-325
379GLBR-337
379GLBR-340
379GLBR-342
379GLBR-344
379GLBR-350
379GLBR-351
379GLBR-352
379GLBR-357
379GLBR-360
379GLBR-19
379GLBR-24
379GLBR-46
379GLBR-46-R
379GLBR-51
379GLBR-53
379GLBR-376. Rep 1
379GLBR-376, Rep 2
379GLBR-376. Rep 3
379GLBR-378
379GLBR-380
379GLBR-384
379GLBR-388
379GLBR-388-R
379GLBR-395
379GLBR-396
379GLBR-397
Naph- Acenaph- Acenaph- Dibenzo-
Sponsor ID thalene thylene thene Flourene thiophene
I BIN C I
19NOV4:504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV1:003SC3O
20NOV1.-553SC3O
20NOV3:154SC3O
20NOV3-.154SC3O
20NOV3:154SC3O
20NOV3:337SC3O
20NOV3278SC3O
I BIN D |
07OCT2:041SDO
07OCT2:121SDO
08OCT5:132SD3O
08OCT5:132SD3O
08OCT5:402SD1O
08OCT5:302SD20
21NOV12:003SD1O
21NOV12:003SD1O
21NOV12:003SD1O
21NOV1:353SD1O
21NOV2:433SD1O
21NOV5:078SD10
21NOV5:107SD1O
21NOV5:107SD1O
21NOV5224SD1O
21NOV5224SD1O
21NOV5224SD1O
17
45
64
53
49
36
19
19
326
36
98
97
1134
58
157
199
61
33
68
237
62
108
103
187
40
14
16
9 U
13
39
37
27
12
14U
15
29
7 U
41
36
498
53
40
57
34
31
31
45
27
9 U
24
46U
5 U
6 U
7 U
16U
19
56
69
44
13
26 U
14U
69 #
12 U
49
43
3656
56
697
616
71
46
54
510
42
15 U
41 #
81 U
8 U
10 U
13 U
12U
48
88
95
71
27
20 U
21
265
19
78
71
4312 D
86
646
599
104
70
79
454
59
37
168
173
7 U
9 U
11 U
18
82
59
74
50
32
24
32
1219
43
49
42
1700
52
397
383
71
55
55
302
39
51
276
289
10
5 U
7 U
Phenan-
threne
147
517
553
761
530
268
235
280
2295 D
211
546
499
33186 D
655
6699 D
5987 D
703
520
522
4506 D
402
299
1455
1785
54
34
29
Anthra-
cene
24
98
112
175
110
42
56
69
290
41
120
106
3081 D
144
1358
1261
173
130
132
360
103
57
267
483
8
5 U
7 U
Fluoran-
thene
345
1205
1076
1585
1102
599
' 622
735
2195 0
416
1352
1360
39360 D
1242
10290 D
9639 D
1426
1067
1117
5568 D
892
709
3825 D
4220
104
76
61
Page 4a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
379GLBR-325
379GLBR-337
379GLBR-340
379GLBR-342
379GLBR-344
379GLBR-350
379GLBR-351
379GLBR-352
379GLBR-357
379GLBR-360
379GLBR-19
379GLBR-24
379GLBR-46
379GLBR-46-R
379GLBR-51
379GLBR-53
379GLBR-376, Rep 1
379GLBR-376, Rep 2
379GLBR-376, Rep 3
379GLBR-378
379GLBR-380
379GLBR-384
379GLBR-388
379GLBR-388-R
379GLBR-395
379GLBR-396
379GLBR-397
Sponsor ID
I BIN C |
19NOV4-.504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV1.-003SC3O
20NOV1:553SC3O
20NOV3:154SC3O
20NOV3:154SC3O
20NOV3:154SC3O
20NOV3337SC3O
20NOV3278SC3O
I BIN 0 |
07OCT2XM1SDO
07G<;T2:121SDO
08OCT5:132SD3O
08OCT5:132SD3O
08OCT5:402SD1O
08OCT5:302SD20
21NOV12:003SD1O
21NOV12:003SD1O
21NOV12:003SD1O
21NOV1:353SD1O
21NOV2:433SD1O
21NOV5:078SD10
21NOV5:107SD1O
21NOV5.-107SD1O
21NOV5224SD1O
21NOV5224SD1O
21NOV5224SD1O
Benzo[a]-
Pyrene anthracene
208
886
851
1156
808
434
448
528
2972 D
315
980
1000
25732 D
946
7635 D
7165 D
1078
824
860
4717 D
673
532
2867 D
3297
75
48
34
148
601
398
599
396
223
276
330
2064 0
235
490
494
13327 D
444
3449 D
3517
543
408
422
2147 D
335
481
1597 D
2155
52
31
23
Benzo(b)- Benzo(k)- BenzofaJ- [1
Chrysene Fluoranthene Fluoranthene pyrene
250
950
555
728
530
378
386
449
4345 0
382
672
696
14210 D
620
3480 D
3367
656
543
548
2736 D
440
784
2794 D
3345
100
56
46
302
1446*
616
828
618
457
476
554
3580 0
533
815
830
13802 D
621
5527 D
3646
805
652
657
2658 D
528
1514
6742
5641
233
60
85
196
773 #
449
614
457
289
316
389
5 U
281
515
527
11813 D
486
2849
2862
533
448
443
1901 D
351
821
6 U
17U
9
32
3 U
112
682
511
596
404
255
279
368
2510 D
274
592
587
5 U
478
3303
3564
632
485
475
2778 D
344
504
1418 *
1616
41
7
4 U
Indeno
,2,3-cd]-
pyrene
160
600
335
465
357
208
261
314
886
243
451
444
7382 D
364
2363
2233
451
376
374
1395
292
559
1386
1147
44
14
12
Page 4b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSLCode
379GLBR-325
379GLBR-337
379GLBR-340
379GLBR-342
379GLBR-344
379GLBR-350
379GLBR-351
379GLBR-352
379GLBR-357
379GLBR-360
379GLBR-19
379GLBR-24
379GLBR-46
379GLBR-46-R
379GLBR-51
379GLBR-53
379GLBR-376. Rep 1
379GLBR-376. Rep 2
379GLBR-376. Rep 3
379GLBR-378
379GLBR-380
379GLBR-384
379GLBR-388
379GLBR-388-R
379GLBR-395
379GLBR-396
379GLBR-397
Sponsor ID
I BINC
19NOV4:504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV1:003SC30
20NOV1:553SC3O
20NOV3:154SC30
20NOV3:154SC30
20NOV3:154SC30
20NOV3337SC3O
20NOV3278SC30
I BIND
07OCT2:041SDO
07OCT2:121SDO
08OCT5:132SD3O
08OCT5:132SD30
08OCT5:402SD10
08OCT5:302SD20
21NOV12:003SD10
21NOV12:003SD10
21NOV12-.003SD10
21NOV1:353SD10
21NOV2:433SD1O
21NOV5:078SD10
21NOV5:107SD1O
21NOV5:107SD1O
21NOV5224SD1O
21NOV5224SD10
21NOV5-224SD10
Dibenzo[a,h]-
anthracene
I
69
245
116
169
99
79
95
115
661
95
I
178
165
2276
92
978
892
164
136
134
581
79
237
593
521
23
8
7
Benzo[ghi]
perylene
160
631
349
447
342
225
251
307
1960
269
412
398
D 6885 D
373
1997
2029
434
363
361
1568
281
603
1538
1273
44
11
8
d8 Naph-
thalene
49%
74%
74%
57%
49%
77%
50%
38% *
72%
64%
81%
90%
87%
73%
38% *
93%
50%
18% '
48%
78%
55%
75%
66%
72%
69%
52%
50%
% Surrogate
Recovery
d10 Acena- D10-
phthene Fluorene
40%
71%
70%
54%
42%
73%
46%
38% *
71%
65%
67%
72%
65%
97%
32% *
76%
54%
42%
42%
72%
43%
71%
72%
101%
67%
32% *
27% *
60%
88%
90%
89%
74%
95%
72%
81%
92%
83%
95%
104%
99%
89%
50%
117%
94%
77%
80%
92%
86%
88%
93%
85%
84%
73%
65%
D14 Dibenzo-
(a,h)Anthracene
71%
105%
100%
114%
94%
109%
85%
97%
131% *
95%
131% *
133% *
114%
99%
66%
162% *
112%
106%
95%
104%
105%
128% *
161% *
103%
89%
40%
41%
Page 4c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
Naph- Acenaph- Acenaph- Dibenzo-
MSLCode Sponsor ID thalene thylene thene Flourene thiophene
Blank-1
Blank-2
Blank-3
Blank-4
Blank-5
Blank-R
Blank-Diluted
STANDARD REFERENCE MATERIAL
SRM-1 (HS-2) (1)
SRM-2 (HS-2)
SRM-3 (HS-2)
SRM-4 (HS-2)
SRM-5 (HS-2)
RSD%
NIST 1941. Rep 1
NIST 1941. Rep 2
NIST 1941, Rep 3
certified value
57
22
14 U
16
46
16
91 U
250
138
92
154
201
36%
872
75 U
177
NA
7 U
20 U
11 U
12U
8 U
7 U
80U
157
148
136
123
151
10%
82
140
117
NA
12U
34 U
20 U
22 U
13U
13 U
134 U
97
87
62
68
78
18%
44 U
112U
66 U
NA
9 U
27 U
16U
20 U
11 U
9 U
99 U
209
175
177
174
225
12%
78
46
64
NA
7 U
18 U
10 U
13 U
8 U
7 U
70 U
221
188
179
172
225
12%
66
64
71
NA
Phenan- Anthra-
threne cene
6
15U
8 U
11 U
7
6
55 U
2750
2495
2411 E
2181
2916 E
11%
519
514
574
577
±39
6 U
17U
10 U
13 U
8 U
6 U
70 U
278
269
243
212
307
14%
185
193
207
202
±42
Fluoran-
thene
8
12 U
7 U
11 U
8
5 U
53 U
'
6622
5588
5811 E
5451 E
6482 E
9%
1098
1097
1202
1220
±240
Page 5a
-------
BUFFALO RIVER PILOT PROJECT (*379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSLCode Sponsor 10
Blank-1
Blank-2
Blank-3
Blank-4
Blank-5
Blank-R
Blank-Diluted
STANDARD REFERENCE MATERIAL
SRM-1 (HS-2) (1)
SRM-2 (HS-2)
SRM-3 (HS-2)
SRM-4 (HS-2)
SRM-5 (HS-2)
RSD%
NIST 1941, Rep 1
NIST 1941, Rep 2
NIST 1941, Rep 3
certified value
Indeno
Benzo[a]- Benzo(b)- Benzo(k)- Benzo[aJ- [1r2.3-cdJ-
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene pyrene
5 U
11 U
6 U
10U
9
5 U
48U
4121
3513
3501 E
3375 E
4127 E
10%
938
940
1024
1080
±200
5 U
10U
6 U
10U
5
4 U
45 U
1800
1568
1642
1447
1770 E
9%
435
450
488
550
±79
5 U
9 U
5 U
9 U
11
4 U
42 U
2170
1930
1919 E
1704 E
2217 E
11%
590
612
663
NA
NA
5 U
9 U
6 *
9 U
13
5
42 U
2024
1765
2118 E
1745
2487 E
15%
825
842
935
780
±190
4 U
8 U
4 U
8 U
7
3U
36 U
1415
1510
1506
1404
1798
10%
611
603
638
444
±49
5 U
9 U
6 U
10U
5 U
4 U
45 U
793
971
973
986
1159
13%
457
460
499
670
±130
3 U
6 U
4 U
6 U
5
3 U
26 U
867
779
894
759
925
9%
453
440
487
569
±40
Page 5b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code Sponsor ID
Blank-1
Blank-2
Blank-3
Blank-4
Blank-5
Blank-R
Blank-Diluted
STANDARD REFERENCE MATERIAL
SRM-1 (HS-2) (1)
SRM-2 (HS-2)
SRM-3 (HS-2)
SRM-4 (HS-2)
SRM-5 (HS-2)
N1ST 1941, Rep 1
NIST 1941, Rep 2
NIST 1941, Rep 3
certified
Dibenzo[a,h]-
anthracene
4
7
4
7
4
3
32
365
295
358
303
357
RSD% 10%
142
139
156
value NA
NA
Benzo[ghi]
perylene
U 4 U
U 6 U
U 4 U
U 7 U
U 5
U 3 U
U 28 U
850
682
711
653
896
14%
463
454
501
516
±83
d8 Naph-
thalene
71%
63%
1%*
51%
71%
72%
0%*
71%
58%
46%
72%
71%
NA
64%
0%*
9%*
NA
NA
% Surrogate
Recovery
d10 Acena- 010-
phthene Fluorene
1% *
31% *
14%*
12% *
67%
81%
14%*
53%
30%*
29% *
63%
68%
NA
78%
68%
85%
NA
NA
84%
71%
46%
71%
85%
79%
40%
81%
66%
79%
78%
88%
NA
73%
49%
66%
NA
NA
014 Dibenzo-
(a.h)Anthracene
16%
62%
62%
50%
96%
76%
48%
91%
74%
92%
95%
113%
NA
71%
75%
86%
NA
NA
Page 5c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode Sponsor ID
SPIKE RESULTS
Amount Spiked
Blank-4
Blank-4 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5+ Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Naph- Acenaph- Acenaph- Dibenzo- Phenan- Anthra-
thalene thylene thene Flourene thiophene threne cene
167
16
120
104
62%
167
46
168
123
73%
167
46
88
42
25% *
167
16
138
122
73%
167
16
137
121
72%
167
12U
53
53
32%*
167
8 U
139
139
83%
167
8 U
107
107
64%
167
7 U
124
124
74%
167
7 U
135
135
81%
167
22 U
103
103
62%
167
13U
151
151
90%
167
13 U
118
118
71%
167
13 U
141
141
84%
167
13 U
152
152
91%
167
20 U
133
133
80%
167
11 U
161
161
96%
167
11 U
128
128
77%
167
9 U
135
135
81%
167
9 U
148
148
89%
167
13 U
81
81
49%
167
8 U
146
146
87%
167
8 U
118
118
71%
167
7 U
152
152
91%
167
7 U
158
158
95%
167
11 U
137
137
82%
167
7
159
152
91%
167
7
130
123
74%
167
6
166
160
96%
167
6
169
163
98%
167
13U
44
44
26%*
167
8 U
107
107
64%
167
8 U
93
93
56%
167
6 U
153
153
92%
167
6 U
145
145
87%
Fluoran-
thene
167
11 U
187 E
187 E
112%
167
8
186
178
107%
167
8
158
150
90%
167
5 U
171
171
103%
167
5 U
176
176
105%
Page 6a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode Sponsor ID
SPIKE RESULTS
Amount Spiked
Blank-4
Blank-4 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5+ Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5-t- Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Benzo[a]- Benzo(b)- Benzo(k)- Benzo[a]- [1
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
167
10U
148 E
148 E
102%
167
9
168
160
96%
167
9
144
135
81%
167
5 U
168
168
100%
167
5 U
167
167
100%
167
10 U
130
130
78%
167
5
150
145
87%
167
5
134
129
77%
167
4 U
157
157
94%
167
4 U
158
158
95%
167
9 U
147
147
88%
167
1 1
155
144
86%
167
11
136
125
75%
167
4 U
159
159
95%
167
4 U
161
161
96%
167
9 U
195
195
117%
167
13
220
207
124% *
167
13
187
175
105%
167
5
167
162
97%
167
5
186
167
100%
167
8 U
186
186
111%
167
7
210
203
121%*
167
7
189
181
109%
167
3 U
167
167
100%
167
3 U
187
187
112%
167
10 U
11 U
11 U
NA
167
5 U
136
136
82%
167
5 U
122
122
73%
167
4 U
140
140
84%
167
4 U
139
139
83%
Indeno
,2.3-cdJ-
pyrene
167
6 U
121
121
72%
'167
5
117
112
67%
167
5
127
123
73%
167
3 U
164
164
98%
167
3 U
178
178
107%
Page 6b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSLCode Sponsor ID
SPIKE RESULTS
Amount Spiked
Blank-4
Blank-4 -»• Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5-t- Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-5
Blank-5+ Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
Blank-R
Blank-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Dibenzo(a,h]- Benzo[ghi]
anthracene perylene
167 167
7 U 7 U
173 91
173 91
104% 55%
167 167
4 U 5
170 117
170 112
102% 67%
167 167
4 U 5
142 97
142 92
85% 55%
167 167
3 U 3 U
145 127
145 127
87% 76%
167 167
3 U 3 U
160 138
160 138
96% 83%
d8 Naph-
thalene
NA
51%
49%
NA
NA
NA
71%
62%
NA
NA
NA
71%
31%*
NA
NA
NA
72%
71%
NA
NA
NA
72%
70%
NA
NA
% Surrogate
Recovery
d10 Acena- D10-
phthene Fluorene
NA
12%*
42%
NA
NA
NA
67%
61%
NA
NA
NA
67%
57%
NA
NA
NA
81%
82%
NA
NA
NA
81%
83%
NA
NA
NA
71%
66%
NA
NA
NA
85%
78%
NA
NA
NA
85%
75%
NA
NA
NA
79%
83%
NA
NA
NA
79%
85%
NA
NA
D14 Dibenzo-
(a,h) Anthracene
NA
50%
78%
NA
NA
NA
96%
88%
NA
NA
NA
96%
85%
NA
NA
NA
76%
84%
NA
NA
NA
76%
88%
NA
NA
Page 6c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
Naph- Acenaph- Acenaph- Dibenzo-
MSLCode Sponsor ID thalene thylene thene Flourena thiophene
SPIKE RESULTS
Amount Spiked
379GLBR-1 1 1 -R 22OCT5:563SA2O
379GLBR-1 1 1 -R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-1 1 1 -R 22OCT5:563SA2O
379GLBR-111-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31OCT2:384SB3O
379GLBR-247 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31OCT2:384SB3O
379GLBR-247 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247-R 31OCT2:384SB3O
379GLBR-247-R + Spike
Amount Recovered
Percent Recovery
303
36 U
272
262
87%
312
36 U
94
94
30%'
98
21
73
52
53%
100
21
67
46
46%
154
45 U
139
139
90%
303
44
277
233
77%
312
44
314
270
87%
98
12U
47
47
48%
100
12U
40
40
40%
154
39U
93
93
60%
303
53 U
314
314
104%
312
53 U
396
396
127%*
98
22 *
189*
167
170% *
100
22*
166
144
145%*
154
68 U
131
131
85%
303
46
310
264
87%
312
46
305
260
83%
98
14 U
69
69
70%
100
14 U
63
63
63%
154
9 U
127
127
82%
303
32
326
294
97%
312
32
347
315
101%
98
16
76
60
61%
100
16
76
60
60%
154
21
147
126
82%
Phenan-
threne
303
446
767
321
106%
312
446
1128
683
219% *
98
90
157
67
68%
100
90
139
49
49%
154
141
261
119
77%
Anthra-
cene
303
93
382
289.
96%
312
93
426
333
107%
98
13
54
41
42%
100
13
52
39
39% *
154
18
127
109
71%
Fluoran-
thene
303
978
1333
355
117%
312
978
2111
1132
363% *
98
166
255
89
91%
100
166
210
44
44%
154
171
359
187
122% *
Page 7a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode Sponsor ID
SPIKE RESULTS
Amount Spiked
379GLBR-1 1 1 -R 22OCT5:563SA2O
379GLBR-111-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-1 1 1 -R 22OCT5:563SA2O
379GLBR-111-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31OCT2:384SB3O
379GLBR-247 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31 GOT2:384SB30
379GLBR-247 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247-R 31OCT2:384SB3O
379GLBR-247-R + Spike
Amount Recovered
Percent Recovery
Benzo[a]- Benzo(b)- Benzo(k)- Benzo[a)- [1
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
303
737
1069
332
109%
312
737
1654
916
294% *
98
109
177
68
69%
100
109
152
43
43%
154
121
278
157
102%
303
339
643
304
100%
312
339
1009
671
215%*
98
73
142
69
70%
100
73
123
50
50%
154
87
215
129
84%
303
487
795
308
102%
312
487
1277
790
253% *
98
132
207
75
77%
100
132
174
42
42%
154
156
282
126
82%
303
507
849
342
113%
312
507
1264
757
243% *
98
253
225
-28
-29% *
100
253
184
-69
-69% *
154
262
309
47
31% *
303
373
664
290
96%
312
373
1031
657
211%*
98
4 U
171
171
174% *
100
4 U
141
141
142% *
154
3 U
237
234
152% *
303
372
643
270
89%
312
372
977
604
194%*
98
53
50
-3
-3%*
100
53
32
-21
-21%*
154
60
154
94
61%
Indeno
,2.3-cd]-
pyrene
303
294
632
339
112%
312
294
844
550
176% *
98
67
118
51
52%
100
67
83
16
16%'
154
59
165
107
69%
Page 7b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSLCode Sponsor ID
SPIKE RESULTS
Amount Spiked
3790LBR-111-R 22OCT5:563SA2O
379GLBR-111-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-111-R 22OCT5:563SA2O
379GLBR-111-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31 OCT2:384SB3O
379GLBR-247 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247 31OCT2:384SB3O
379GLBR-247 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-247-R 31OCT2:384SB3O
379GLBR-247-R + Spike
Amount Recovered
Percent Recovery
Dibenzo[a,h]-
anthracene
303
74
404
330
109%
312
74
506
432
139% *
98
32
97
65
66%
100
32
78
46
46%
154
30
136
106
69%
Benzo[ghi]
perylene
303
294
579
285
94%
312
294
759
465
149% *
98
64
92
28
29%*
100
64
61
-3
-3% '
154
62
142
80
52%
d8 Naph-
thalene
MA
33% *
67%
NA
MA
NA
33% *
21%*
NA
NA
NA
50%
50%
NA
NA
NA
50%
43%
NA
NA
NA
1% *
67%
NA
NA
% Surrogate
Recovery
d10 Acena- D10-
phthene Fluorene
NA
72%
85%
NA
NA
NA
72%
95%
NA
NA
NA
39% *
45%
NA
NA
NA
39% '
40%
NA
NA
NA
131% '
75%
NA
NA
NA
65%
83%
NA ..
NA
NA
65%
75%
NA
NA
NA
55%
58%
NA
NA
NA
55%
53%
NA
NA
NA
52%
74%
NA
NA
D14 Dibenzo-
(a.h)Anthracene
NA
91%
95%
NA
NA
NA
91%
95%
NA
NA
NA
63%
63%
NA
NA
NA
63%
55%
NA
NA
NA
67%
63%
NA
NA
Page 7c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
Naph- Acenaph- Acenaph- Dibenzo-
MSLCode Sponsor ID thalene thylene thane Flourene thiophene
SPIKE RESULTS
Amount Spiked
379GLBR-247-R 31OCT2:384SB3O
379GLBR-247-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268 1NOV10:208SB3O
379GLBR-268 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268 1 NOV10:208SB3O
379GLBR-268 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388 21NOV5:107SD1O
379GLBR-388 + Spike
Amount Recovered
Percent Recovery
142
45 U
34 U
NA
NA
109
81
133
52
48%
96
81
141
59
62%
107
103
186
83
78%
142
39U
97
97
69%
109
8 U
61
61
56%
96
8 U
56
56
58%
107
24
112
88
82%
142
68 U
193
193
136%*
109
15 U
82
82
76%
96
15 U
80
80
83%
107
41 #
140
99
93%
142
9 U
79
79
55%
109
34
112
78
71%
96
34
123
88
92%
107
168
281
113
1 05%
142
21
151
130
92%
109
74
142
68
62%
96
74
154
80
83%
107
276
352
76
71%
Phenan- Anthra-
threne cene
142
141
282
141
99%
109
364
390
26
24% *
96
364
444
80
84%
107
1455
1501 D
46
43%
142
18
129
111 .
78%
109
60
101
41
38% *
96
60
111
51
53%
107
267
311
45
42%
Fluoran-
thene
142
171
341
170
120%
109
763
757
-6
-6%*
96
763
865
102
106%
107
3825 D
3923 D
98
92%
Page 8a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concontrations in ng/g)
MSLCode
SPIKE RESULTS
Amount Spiked
379GLBR-247-R
Sponsor ID
31OCT2:384SB3O
379GLBR-247-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268
379GLBR-268 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268
379GLBR-268 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388
379GLBR-388 + Spike
Amount Recovered
Percent Recovery
1NOV10:208SB3O
1NOV10:208SB3O
DUPLICATE
21NOV5:107SD1O
Benzo(a)- Benzo(b)- Benzo(k)- Benzo[a]- [1
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
142
121
270
149
105%
109
475
495
20
18% *
96
475
559
84
88%
107
2867 D
2954 D
87
81%
142
87
213
127
89%
109
360
395
35
32%*
96
360
435
75
78%
107
1597 D
1695 D
98
92%
142
156
289
132
93%
109
562
563
1
1%*
96
562
637
75
78%
107
2794 D
2921 D
127
119%
142
262
303
41
29%*
109
806
760
-47
-43% *
96
806
878
72
75%
107
6742
7409
667
623% *
142
3 U
229
227
160%*
109
422*
479
57
52%
96
422*
506
84
88%
107
6 U
5 U
5
MA
142
60
149
89
62%
109
281
264
-18
-16%'
96
281
282
1
1%*
107
1418#
1572 #
154
144% *
Indeno
,2,3-cdJ-
pyrene
142
59
163
105
74%
109
249
300
51
47%
96
249
323
74
77%
107
1386
1655
269
251% *
Page 8b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
Dibenzo[a,h]- Benzo[ghi]
MSLCode Sponsor ID anthracene perylene
SPIKE RESULTS
Amount Spiked 142 142
379GLBR-247-R 31OCT2:384SB3O 30 62
379GLBR-247-R + Spike DUPLICATE 130 139
Amount Recovered 100 77
Percent Recovery 70% 54%
Amount Spiked 1 09 109
379GLBR-268 1NOV10:208SB3O 108 224
379GLBR-268 + Spike 209 243
Amount Recovered 101 19
Percent Recovery 92% 18% *
Amount Spiked 96 96
379GLBR-268 1NOV10:208SB30 108 224
379GLBR-268 + Spike DUPLICATE 222 267
Amount Recovered 114 44
Percent Recovery 119% 45%
Amount Spiked 107 107
379GLBR-388 21NOV5:107SD1O 593 1538
379GLBR-388 + Spike 943 1778
Amount Recovered 350 240
Percent Recovery 327% * 224% *
% Surrogate Recovery
d8 Naph- d10 Acena- D10- D14 Dibenzo-
thalene phthene Fluorene (a.h)Anthracene
NA MA MA NA
1% * 131% * 52% 67%
1%* 118% 51% 70%
NA NA NA NA
NA NA NA NA
NA NA NA NA
61% 31% * 71% 64%
56% 52% 68% 76%
NA NA NA NA
NA NA NA NA
NA NA NA NA
61% 31% * 71% 64%
63% 56% 82% 85%
NA NA NA NA
NA NA NA NA
NA NA NA NA
66% 72% 93% 161%
71% 72% 92% 167%
NA NA NA NA
NA NA NA NA
Page 8c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
Naph- Acenaph- Acenaph- Dibenzo-
MSLCode Sponsor ID thalene thylene thene Flourene thiophene
SPIKE RESULTS
Amount Spiked
379GLBR-388 21NOV5:107SD1O
379GLBR-388 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R 21NOV5:107SD1O
379GLBR-388-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R 21NOV5:107SD1O
379GLBR-388-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
REPLICATE ANALYSIS
379GLBR-182. Rep 1 25OCT2:294SB1O
379GLBR-182, Rep 2 25OCT2:294SB1O
379GLBR-182, Rep 3 25OCT2:294SB1O
RSD%
379GLBR-199, Rep 1 20OCT3:573SB2O
379GLBR-199. Rep 2 20OCT3:573SB2O
379GLBR-199, Rep 3 20OCT3:573SB2O
RSD%
117
103
194
91
77%
500
187
549
362
72%
385
187
378
191
50%
27
22
26
11%
62
49
59
12%
117
24
126
101
87%
500
46 U
470
470
94%
385
46U
325
325
84%
7 U
11 U
11 U
NA
31
29
23
15%
117
41 *
160
118
101%
500
81 U
547
547
109%
385
81 U
390
390
101%
12 U
69 #
72 #
4%
52
42
40
14%
117
168
296
128
110%
500
173
661
488
98%
385
173
511
338
88%
16
21
16
16%
74
59
61
13%
117
276
370
95
81%
500
289
800
511
102%
385
289
664
375
97%
11
18
14
25% *
48
40
44
10%
Phenan- Anthra-
threne cene
117
1455
1503 D
48
41%
500
1785
2263
478
96%
385
1785
2080
295
77%
146
191
143
17%
503
424
472
9%
117
267
316
49.
42%
500
483
915
432
86%
385
483
777
294
76%
18
35
29
32% *
91
81
93
7%
Fluoran-
thene
117
3825 D
3853 D
28
24% *
500
4220
4951
732
146% *
385
4220
4828
609
158% *
274
356
277
15%
1123
931
892
13%
Page 9a
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSLCode
SPIKE RESULTS
Amount Spiked
379GLBR-386
379GLBR-388 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R
Sponsor ID
21NOV5:107SD1O
DUPLICATE
21NOV5:107SD1O
379GLBR-388-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R
21NOV5:107SD1O
379GLBR-388-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
REPLICATE ANALYSIS
379GLBR-182. Rep 1
379GLBR-182, Rep 2
379GLBR-182. Rep 3
379GLBR-199. Rep 1
379GLBR-199, Rep 2
379GLBR-199. Rep 3
25OCT2:294SB1O
25OCT2:294SB1O
25OCT2:294SB1O
RSD%
20OCT3:573SB2O
20OCT3:573SB2O
20OCT3:573SB2O
RSD%
Benzo[a]- Benzo(b)- Benzo(k)- Benzo[a]- [1
Pyrene anthracene Chrysene Fluoranthene Fluoranthene pyrene
117
2867 D
2927 D
60
51%
500
3297
3889
592
118%
385
3297
3805
508
132%*
173
254
196
20%
833
696
649
13%
117
1597 D
1682 D
85
73%
500
2155
2583
428
86%
385
2155
2484
329
85%
98
145
122
19%
376
322
298
12%
117
2794 D
2925 D
131
112%
500
3345
3543
198
40%
385
3345
3547
201
52%
187
217
195
8%
517
433
410
12%
117
6742
7141 E
399
341% *
500
5641
3969 #
-1672
-334% *
385
5641
3889 #
-1752
-455% *
243
239
231
3%
631
499
470
16%
117
6 U
5 U
5
NA
500
17 U
2271 #
2271 #
454% *
385
17 U
2005 #
2005
521% *
147
154
137
6%
457
378
335
16%
117
1418#
1545*
127
108%
500
1616
1965
348
70%
385
1616
1876
260
67%
29
97
94
52% *
447
383
343
13%
Indeno
,2.3-cd]-
pyrene
117
1386
1573
187
160% *
500
1147
1701
555
111%
385
1147
1563
416
108%
104
107
100
3%
355
295
268
15%
Page 9b
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
Dibenzo[a.h]-
MSLCode Sponsor ID anthracene
SPIKE RESULTS
Amount Spiked
379GLBR-388 21NOV5:107SD1O
379GLBR-388 + Spike DUPLICATE
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R 21NOV5:107SD1O
379GLBR-388-R + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388-R 21NOV5:107SD1O
379GLBR-388-R + Spike DUPLICATE
Amount Recovered
Percent Recovery
REPLICATE ANALYSIS
379GLBR-182, Rep 1 25OCT2:294SB1O
379GLBR-182. Rep 2 25OCT2:294SB1O
379GLBR-182. Rep 3 25OCT2:294SB1O
RSD%
379GLBR-199, Rep 1 20OCT3:573SB2O
379GLBR-199, Rep 2 20OCT3:573SB2O
379GLBR-199, Rep 3 20OCT3:573SB2O
RSD%
117
593
914
322
275% *
500
521
1067
546
109%
385
521
952
431
112%
48
51
48
4%
130
106
96
16%
Benzo[ghi]
perylene
117
1538
1700
162
138% *
500
1273
1748
476
95%
385
1273
1657
384
100%
90
99
96
5%
353
291
253
17%
d8 Naph-
thalene
NA
66%
63%
NA
NA
NA
72%
77%
NA
NA
NA
72%
63%
NA
NA
62%
47%
66%
NA
87%
74%
70%
NA
% Surrogate
Recovery
d10 Acena- 010-
phthene Fluorene
NA
72%
69%
NA
NA
NA
101%
91%
NA
NA
NA
101%
81%
NA
NA
45%
43%
62%
NA
73%
62%
61%
NA
NA
93%
87%
NA
NA
NA
85%
92%
NA
NA
NA
85%
83%
NA
NA
78%
64%
78%
NA
94%
78%
78%
NA
D14 Dibenzo-
(a,h)Anthracene
NA
161%
154%
NA
NA
NA
103%
109%
NA
NA
NA
103%
108%
NA
NA
89%
73%
87%
NA
105%
87%
89%
NA
Page 9c
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
Naph- Acenaph- Acenaph- Dibenzo-
MSLCode Sponsor ID thalene thylene thene Flourene thiophene
REPLICATE ANALYSIS
379GLBR-18. Rep 1 07OCTT.331SCO
379GLBR-18. Rep 2 07OCT1:331SCO
379GLBR-18, Rep 3 07OCT1:331SCO
RSD%
379GLBR-323. Rep 1 19NOV4:504SC2O
379GLBR-323, Rep 2 19NOV4:504SC2O
379GLBR-323, Rep 3 19NOV4:504SC2O
RSD%
379GLBR-376, Rep 1 21NOV12:003SD1O
379GLBR-376, Rep 2 21NOV12:003SD1O
379GLBR-376, Rep 3 21NOV12:003SD1O
RSD%
* - Recoveries outside of QC limits.
U » Detected at or below detection limit.
R • Rerun samples.
D • Sample diluted 1:10.
E - Value out of calibration range.
147
94
125
22%*
36
31
31
9%
61
33
68
34% *
66
41
53
23% *
7 U
10
7 U
NA
34
31
31
6%
92
67
91
17%
12U
10 U
11 U
NA
71
46
54
22% *
147
95
131
21%*
10U
13
9 U
NA
104
70
79
21% *
105
75
100
17%
24
28
22
12%
71
55
55
15%
Phenan-
threne
923
615
835
20%
128
174
125
19%
703
520
522
18%
Anthra-
cene
264
167
237
23% *
20
28
20
21% *
173
130
132
17%
Fluoran-
thene
1938
1343
1793
18%
. 267
379
265
22% *
1426
1067
1117
16%
# • Ion ratio out of specification.
(1) - HS-2 is not certified for PAHs. However. RSD values give an indication
of relative precision of PAH measurements between batches.
NA • Not applicable/analyzed.
RSD% - Relative Standard Deviation
Page lOa
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
(Concentrations in ng/g)
MSI Code
Sponsor
ID
Pyrene
Benzo[aj-
anthracene
Chrysene
Benzo(b)-
Fluoranthene
Benzo(k)-
Fluoranthene
Benzo[a]-
pyrene
[1
Indeno
,2,3-cd]-
pyrene
379GLBR-18, Rep 1
379GLBR-18, Rep 2
379GLBR-18, Rep 3
379GLBR-323, Rep 1
379GLBR-323, Rep 2
379GLBR-323, Rep 3
379GLBR-376, Rep 1
379GLBR-376, Rep 2
379GLBR-376, Rep 3
07OCT1:331 SCO 1554 785
07OCT1:331SCO 1077 528
07OCT1;331SCO 1436 747
RSD% 18% 20%
19NOV4:504SC2O 189 131
19NOV4:504SC2O 277 178
19NOV4:504SC2O 180 126
RSD% 25%* 20%
21NOV12:003SD10 1078 543
21NOV12:003SD10 824 408
21NOV12:003SD10 860 422
RSD% 15% 16%
957
664
893
18%
238
296
240
13%
656
543
548
11%
1039
766
1033
16%
484
361
308
24%
805
652
657
12%
777
513
695
20%
4 U
229
174
27% *
533
448
443
11%
912
601
852
21%
131
189
123
24%
632
485
475
17%
621
438
583
18%
137
180
141
16%
451
376
374
11%
* - Recoveries outside of QC limits.
U - Detected at or below detection limit.
R • Rerun samples.
D - Sample diluted 1:10.
E - Value out of calibration range.
* - Ion ratio out of specification.
(1) - HS-2 is not certified for PAHs. However, RSD values give an indication
of relative precision of PAH measurements between batches.
NA - Not applicable/analyzed.
RSD% « Relative Standard Deviation
Page lOb
-------
BUFFALO RIVER PILOT PROJECT (#379)
PAH ANALYSIS IN SEDIMENT SAMPLES
MSI Code
Sponsor ID
Dibenzo[a,h]-
anthracene
Benzo(ghi)
perylene
% Surrogate Recovery
d8 Naph-
thalene
d10 Acena-
phthene
D10-
Fluorene
D14 Dibenzo-
(a.h)Anthracene
REPLICATE ANALYSIS
379GLBR-18. Rep 1
379GLBR-18, Rep 2
379GLBR-18, Rep 3
379GLBR-323, Rep 1
379GLBR-323, Rep 2
379GLBR-323, Rep 3
379GLBR-376, Rep 1
379GLBR-376, Rep 2
379GLBR-376, Rep 3
07OCT1:331SCO 251 602
07OCT1:331SCO 179 388
07OCT1:331SCO 241 505
RSD% 18% 22%
19NOV4:504SC2O 54 144
19NOV4:504SC2O 71 189
19NOV4:504SC2O 55 146
RSD% 15% 16%
21NOV12:003SD1O 164 434
21NOV12:003SD1O 136 363
21NOV12:003SD1O 134 361
RSD% 11% 11%
64%
57%
72%
NA
86%
84%
83%
NA
50%
18%
38%
NA
59%
61%
68%
NA
77%
76%
74%
NA
54%
42%
42%
NA
89%
84%
96%
NA
89%
91%
88%
NA
94%
77%
80%
NA
123%
121%
133%
NA
96%
101%
99%
NA
112%
106%
95%
NA
* « Recoveries outside of QC limits.
U - Detected at or below detection limit.
R - Rerun samples.
D • Sample diluted 1:10.
E - Value out of calibration range.
* - Ion ratio out of specification.
(1) - HS-2 is not certified for PAHs. However, RSD values give an indication
of relative precision of PAH measurements between batches.
NA • Not applicable/analyzed.
RSD% - Relative Standard Deviation
Page lOc
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN WATER SAMPLES
Concentrations in ng/L
% Surrogate Recovery
MSL Code
379GLBR-97
379GLBR-97 -
379GLBR-97 ~
379GLBR-128
379GLBR-132
379GLBR-160
379GLBR-161
379GLBR-164
379GLBR-204
379GLBR-187
379GLBR-226
379GLBR-227
379GLBR-252
379GLBR-253
379GLBR-256
379GLBR-257
379GLBR-286
379GLBR-326
379GLBR-331
379GLBR-331 DUP 1
379GLBR-331 DUP 2
379GLBR-361
379GLBR-366
379GLBR-370
Oil.
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(V.10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
(1:10)
Sponsor ID
| BIN A
21OCT6:1810LA1O
21OCT6:2010LA1O
21OCT6:2010LA10
23OCT4:459LA20
23OCT5-2010LA2O
25OCT10.1810LA3O
25OCT10:1910LA3O
25OCT9.549LA3O
30OCT4.206LA3O
| BIN B
25OCT3:0810LB1O
31OCT10:129LB2O
31OCT10:2310LB2O
31OCT3:119LB3O
31OCT3:109LB30
31OCT3:0110LB30
31OCT3:0010LB3O
| BIN C
18NOV5:559LC10
19NOV5:509LC20
19NOV5:0510LC20
19NOV5:0510LC2O
19NOV5:0510LC2O
20NOV2:193LC3O
20NOV2:419LC3O
20NOV3:0110LC3O
Sample
Amount (L)
0.810
0.800
0.800
0.720
0.675
0.700
0.760
0.650
0.800
0.750
0.850
0.825
0.825
0.775
0.750
0.650
0.775
0.800
0.650
0.785
0.800
0.800
0.800
0.726
Aroclor
1242/1248
21,111 D
26.368
22,742 D
24,698 D(a)
60,890 D
21,020 D
33,666 D
69,074 D
200 U
27,605 D
2,000 U
2,000 U
2,000 U
2.000 U
8,107 D
16,922 D
25,956 D
39,269 D
17,890 D
11,157 D
8,028 D
200 U
5,814 D
19,471 D
Page 1
Aroclor
1254
500 U
50 U
500 U
500 U
5,294 E
500 U
500 U
500 U
50 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
50 U
500 U
500 U
Aroclor
1260
500 U
50 U
500 U
500 U
500 U
500 U
500 U
500 U
50 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
500 U
50 U
500 U
500 U
Tetrachloro-
m-Xylene
36.1% '
52.9%
113.4%
103.1% _,
53.0%
113.6%
135.7% '
69.7%
76. 1 %
103.0%
54.6%
66.6%
113.5%
92.3%
72.5%
69.7%
116.9%
65.8%
61.8%
63.1%
56.2%
38.8% *
63.6%
42.6%
Octachloro-
naphthalene
25.7%
38.6%
77 4%
33.3%
36.6%
77.9%
68 5%
59.2%
105 0%
83.3%
33. 1 %
45.4%
58.4%
50.0%
55.5%
47.9%
47.9%
44.5%
54.9%
58.3%
53.8%
52.8%
50.3%
51.8%
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN WATER SAMPLES
379GL8R-275
Concentrations in ng/L
% Surrogate Recovery
MSLCode
379GLBR-398
379GLBR-404
Oil.
(1:10)
(1:10)
Sponsor ID
BIN D
21NOV3:2610LD1O
21NOV4:169LD10
DILUTION WATER
Sample
Amount (L)
0 757
0.705
Aroclor
1242/1248
5,304 D
7.193 D
Aroclor
1254
500 U
500 U
Aroclor
1260
500 U
500 U
Tetrachloro-
m-Xylene
45.7%
49.4%
Octachloro-
naphthalene
51.3%
27.3%
6NOV12:003LO
0 825
200 U
50 U
50 U
36.8% '
59.3%
379GLBR METHOD BLANK
0.500
200 U
50 U
50 U
62.4%
96.4%
MATRIX SPIKE RESULTS
Amount Spiked
380GLBR-132
380GLBR-132 + Spike
Amount Recovered
Percent Recovery
(1:10) 230CT5:2010LA2O
NS
MS
NS
NS
NS
7,143
5,294 E
13,287
7,993
112%
NS
NS
NS
NS
NS
NA
53.0%
43.6%
NA
NA
NA
36.6%
49 5%
NA
NA
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN WATER SAMPLES
Concentrations in ng/L
% Surrogate Recovery
MSLCode
Oil.
Sponsor ID
Sample
Amount (L)
Aroclor
1242/1248
Aroclor
1254
Aroclor
1260
Tetrachloro-
m-Xylene
Octachloro-
naphthalene
REPLICATE ANALYSIS
379GLBR-331 (1:10)
379GLBR-331 DUP 1 (1:10)
379GLBR-331 DUP 2 (1:10)
19NOV50510LC2O
19NOV5.0510LC2O
19NOV50510LC2O
RSD%
17.890 D
11.157 D
8,028 D
41% • '
500 U
500 U
500 U
NA
500 U
500 U
500 U
NA
61.8%
63.1%
56.2%
NA
54.9%
58.3%
53.8%
NA
- = Field replicate.
U = Not detected at detection limit shown
D = Results from diluted sample extract
(a) = Aroclor quantified with one peak, other peaks may have been present, but not quantifiable
E = Estimated/most likely due to residual peaks of primary aroclor.
NS = Not spiked.
NA = Not applicable.
* = Recoveries were outside laboratory control limts (40-120%).
" = RSD exceeded QC limit of 20%.
Page 3
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
Concentrations in ng/g dry weight
% Surrogate Recovery
MSI Code
379GLBR-58
379GLBR-104
379GLBR-107
379GLBR-108
379GLBR-123
379GLBR-136
379GLBR-139
379GLBR-145
379GLBR-153
379GLBR-166
379GLBR-167
379GLBR-65
379GLBR-174
379GLBR-181
379GLBR-193
379GLBR-196
379GLBR-199, Rep 1
379GLBR-199, Rep 2
379GLBR-199, Rep 3
379GLBR-210
379GLBR-213
379GLBR-222
379GLBR-243
379GLBR-248
379GLBR-268
379GLBR-269
Sponsor ID
I BIN A
09OCT11:382SA2O
22OCT11:317SA1O
22OCT1V.378SA1O
22OCT4:203SA2O
23OCT4:274SA2O
24OCT10:457SA2O
24OCT10:508SA2O
24OCT6:203SA3O
25OCT9:214SA3O
25OCT9:307SA3O
25OCT9:368SA3O
I BIN B
09OCT9:542SB1O
25OCT12:153SB1O
25OCT2:254SB1O
250CT3-.527SB1O
25OCT3:578SB1O
30OCT3:573SB2O
30OCT3:573SB2O
30OCT3:573SB20
31OCT9:027SB2O
31OCT9:078SB2O
31OCT9:244Sti2O
31OCT11:503SB3O
31OCT2:354SB3O
1NOV10:208SB3O
1NOV10:157SB3O
Extraction
Date
2/19/92
2/19/92
2/19/92
2/19/92
2/19/92
2/19/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/19/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
2/24/92
Dry Wt.
(%)
60.44
65.53
97.72
52.78
99.79
90.15
77.20
56.46
99.12
91.48
99.41
62.26
62.01
99.00
95.93
99.10
63.20
63.20
63.20
87.81
99.79
99.81
62.88
99.60
99.60
97.78
Aroclor
1242
50 U
50 U
SOU
50 U
SOU
50 U
60 U
60 U
60 U
60 U
60 U
SOU
60U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
Aroclor Aroclor Aroclor
1248 1254 1260
55 D
50 U
SOU
50 U
50 U
50 U
60 U
60 U
60U
201
60 U
SOU
104
60 U
327
81
350
92
60 U
319
60 U
60 U
120
60 U
60 U
60 U
25 U 25 U
25 U 25 U
25 U 25 U
25 U 25 U
25 U 25 U
25 U 25 U
35 U 35 U
120 35 U
35 U 35 U
201 35 U
67 35U
Tetrachloro- Octachloro-
m-Xylene naphthalene
83.1%
65.1%
70.8%
71 .2%
93.7%
58.9% .
84.5%
98.2%
81.9%
91 .5%
87.1%
25 U 25 U 76.5%
80 35 U 75.6%
94 35 U 78.9%
262 35 U 90.6%
75 35 U 105.0%
371 35 U 73.3%
96 35 U 68.5%
84 35 U 96.1%
158 35 U 117.1%
35 U 35 U 112.5%
35 U 35 U 65.4%
97 35 U 98.6%
35 U 35 U 70.0%
35 U 35 U 66.7%
176 35 U 100.3%
136.8% *
107.0%
108.2%
106.5%
143.2%
103.0%
133.6% •
142.6% *
141.6%*
125.9% '
124.2% '
149.2% '
125.4% *
119.7%
129.7% *
169.6% *
138.9% *
125.7% '
169.1%*
145.8% *
222.2% *
167.6% *
164.5% *
182.4% *
152.9% *
145.0% *
Page 1
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
Concentrations in ng/g dry weight
% Surrogate Recovery
MSI Code
369GLBR-73
379GLBR-282
379GLBR-288
379GLBR-302
379GLBR-307
379GLBR-311
379GLBR-323, Rep 1
379GLBR-323, Rep 2
379GLBR-323, Rep 3
379GLBR-337
379GLBR-340
379GLBR-350
379GLBR-357
379GLBR-360
379GLBR-46
379GLBR-378
379GLBR-384
379GLBR-388
379GLBR-395
Blank-1
Blank-2
Blank-3
Sponsor ID
BINC
09OCT4:562SC1O
18NOV3:503SC1O
18NOV6:1510LC1O
19NOV8:594SC1O
19NOV9:23ISC1O
19NOV11:303SC2O
19NOV4:504SC2O
19NOV4:504SC2O
19NOV4:504SC2O
20NOV8:157SC2O
20NOV11:443SC3O
20NOV3:154SC3O
20NOV3:337SC3O
20NOV3:278SC3O
BIN D
08OCT5:132SD3O
21NOV1:353SD1O
21NOV5:073SD1O
21NOV5:107SD1O
21NOV5:224D1O
Extraction
Date
I
2/19/92
2/24/92
2/24/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
3/4/92
I
3/4/92
3/4/92
3/4/92
3/4/92
2/19/92
2/24/92
3/4/92
Dry Wt.
(%)
62.20
62.71
73.20
99.66
98.79
69.87
99.79
99.79
99.79
95.62
55.58
95.97
77.29
99.58
60.26
57.63
100.00
93.10
100.00
MA
NA
NA
Aroclor
1242
50 U
60 U
60 U
60U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
60 U
50 U
60 U
60 U
60 U
60 U
50 U
60 U
* 60 U
Aroclor
1248
50 U
232
975
60 U
60 U
209
133
119
114
284
163
109
738
60 U
50 U
320
251
674
60 U
50 U
60 U
60 U
Aroclor
1254
113
35 U
35 U
17
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
500 U * *
35 U
25 U
35 U
35 U
35 U
35 U
25 U
35 U
35 U
Aroclor
1260
25 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
35 U
25 U
35 U
35 U
35 U
35 U
25 U
35 U
35 U
Tetrachloro-
m-Xylene
87.1%
96.0%
104.9%
103.1%
71 .5%
97.1%
97.2%'
101.0%
95.3%
102.6%
67.5%
72.5%
125.7% *
75.8%
76.8%
71 .7%
96.7%
103.6%
86.4%
46.1%
77.7%
86.3%
Octachloro-
naphthalene
125.3% *
175.7% '
137.4% *
115.4%
122.0% '
119.8%
98.5%
96.4%
136.7% '
188.1% '
119.3%
. 143.8% *
90.1%
1 53.3% *
130.3% '
199.9% *
1 04.6%
129.0% *
1 69.3% *
86.5%
146.6% '
1 26.9% '
Page 2
-------
BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
Concentrations in ng/g dry weight
% Surrogate Recovery
Extraction Dry Wt.
MSLCode Sponsor ID Date (%)
STANDARD REFERENCE MATERIAL
SRM-1 HS-2 2/19/92 NA
SRM-2 HS-2 2/24/92 NA
SRM-3 HS-2 3/4/92 NA
certified NA
value NA
SPIKE RESULTS
Amount Spiked
379GLBR-BlanK-2+ Spike DUP
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-Blank-3 3/4/92
379GLBR-Blank-3 Spike DUP
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-Blank-3 3/4/92
379GLBR-Blank-3+ Spike DUP
Amount Recovered
Percent Recovery
Aroclor
1242
50 U
60 U
60 U
N3
NC
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
Aroclor Aroclor Aroclor
1248 1254 1260
50 U 262 25 U
60 U 261 35 U
60 U 381 35 U
NC 111.8 NS
N3 ±2.5 NS
NS 2500 NS
NS 3173 NS
NS 3173 NS
NS 127% • NS
NS 2500 NS
NS 35 U NS
NS 2767 NS
NS 2767 NS
NS 111% NS
NS 2500 NS
NS 35 U NS
NS 5149 NS
NS 5149 NS
NS 206% * NS
Tetrachloro- Octachloro-
m-Xylene naphthalene
67.6% 194.2%
84.0% 114.4%
83.9% 180.9%
NA NA
NA NA
NA NA
60.8% 132.9%
NA NA
NA NA
NA NA
86.3% 126.9%
78.2% 96.2%
NA NA
NA NA
NA NA
86.3% 126.9%
73.8% 243.0%
NA NA
NA NA
Page 3
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BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
Concentrations in ng/g dry weight
% Surrogate Recovery
Extraction Dry Wt.
MSL Code Sponsor ID Date (%)
Amount Spiked
379GLBR-46 08OCT5:132SD3O 2/19/92 60.26
379GLBR-46 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-46 08OCT5:132SD3O 2/19/92 60.26
379GLBR-46 + Spike DUP
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268 1 NOV1 0-.208SB3O 2/24/92 99.60
379GLBR-268 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-268 1 NOV1 0:208SB3O 2/24/92 99.60
379GLBR-268 + Spike DUP
Amount Recovered
Percent Recovery
Aroclor
1242
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
Aroclor Aroclor Aroclor
1248 1254 1260
NS 553 NS
NS 25U NS
NS 455 NS
NS 455 NS
NS 82% NS
NS 714 NS
NS 25 U NS
NS 517 NS
NS 517 NS
NS 72% NS
NS 547 NS
NS 62 NS
NS 732 NS
NS 670 NS
NS 122% * NS
NS 480 NS
NS 62 NS
NS 696 NS
NS 634 NS
NS 132% * NS
Tetrachloro- Octachloro-
m-Xylene naphthalene
NA NA
76.8% 130.3%
83.0% NA
NA NA
NA NA
NA NA
76.8% 130.3%
85.0%' 126.8%
NA NA
NA NA
NA NA
66.7% 152.9%
63.6% 137.6%
NA NA
NA NA
NA NA
66.7% 1 52.9%
75.7% 138.2%
NA NA
NA NA
Page 4
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BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
Concentrations in ng/g dry weight
% Surrogate Recovery
MSLCode Sponsor ID
Amount Spiked
379GLBR-388 21NOV5:107SD1O
379GLBR-388 + Spike
Amount Recovered
Percent Recovery
Amount Spiked
379GLBR-388 21NOV5:107SD1O
379GLBR-388 + Spike DUP
Amount Recovered
Percent Recovery
REPLICATE ANALYSIS
379GLBR-199, Rep 1 30OCT3:573SB2O
379GLBR-199, Rep 2 30OCT3:573SB2O
379GLBR-199, Rep 3 30OCT3:573SB2O
379GLBR-323, Rep 1 19NOV4:504SC2O
379GLBR-323, Rep 2 19NOV4:504SC2O
379GLBR-323, Rep 3 19NOV4:504SC2O
Extraction
Date
3/4/92
3/4/92
2/24/92
2/24/92
2/24/92
RSD%
3/4/92
3/4/92
3/4/92
RSD%
Dry Wt.
(%)
93.10
93.10
63.20
63.20
63.20
99.79
99.79
99.79
Aroclor
1242
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
60 U
60 U
60 U
NA
60 U
60 U
60 U
NA
Aroclor Aroclor Aroclor
1248 1254 1260
NS 534 NS
NS 674 NS
NS 1157 NS
NS 483 NS
NS 90% NS
NS 585 NS
NS 674 NS
NS 1141 NS
NS 467 NS
NS 80% NS
350 371 35 U
92 96 35 U
60 U 84 35 U
117%* 89%* NA
Tetrachloro- Octachloro-
m-Xylene naphthalene
NA NA
103.6% 129.0%
115.8% 106.4%
NA NA
NA NA
NA NA
103.6%. > 129.0%
115.0% 79.0%
NA NA
NA NA
73.3% 138.9%
68.5% 125.7%
96.1% 169.1%
NA NA
133 63 35 U 97.2% 98.5%
119 51 35 U 101.0% 96.4%
114 51 35 U 95.3% 136.7%
8% 13% NA
NA NA
U « Not detected at detection limit shown.
J * Detected below detection limit.
D - Detected Aroclor, but undetected pattern due to low levels.
* * Outside of QC limits.
** « Matrix interference.
NS = Not Spiked. NC - Not certified.
NA « Not Applicable.
RSD % a Relative Standard Deviation.
Page 5
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BUFFALO RIVER PILOT PROJECT (CF *379)
PCB/AROCLORS IN SEDIMENT SAMPLES
TABLE NO. 2
(concentrations in ng/g dry weight)
% Surrogate Recovery
MSLCode
379GLBR-15, Rep 1
379GLBR-15, Rep 2
379GLBR-15, Rep 3
379GLBR-17
379GLBR-21
379GLBR-22
Blank
Sponsor ID
07OCT1:212SCO
07OCT1:212SCO
07OCT1-.212SCO
07OCT1 2:091 SAO
07OCT1 2:531 SBO
070CT1:521SDO
Extraction
Date
10/10/91
10/10/91
10/10/91
10/10/91
10/10/91
10/10/91
10/10/91
Dry Wt.
(%)
59.0
59.0
59.0
57.9
55.2
58.7
MA
Aroclor
1242
73 E
79 E
73 E
20 U
20 U
20 U
20 U
Aroclor Aroclor Aroclor
1248 1254 1260
217 99 E 20 U
236 108 E 20 U
239 20 U . 20 U
85 20 U 20 U
20 U 20 U 20 U
179 E 202 20 U
20 U 20 U 20 U
Tetrachloro- Octachloro-
m-Xylene naphthalene
53.9% 85.1%
56.8% 89.2%
56.9% 95.9%
60.9% 93.2%
66.9% 107.3%
66.7% 100.6%
82.9% 127.4%
STANDARD REFERENCE MATRIAL
SRM-1 (1941)
SPIKE RESULTS
Amount Spiked
379GLBR-22
E79GLBR-22 + Spike
Amount Recovered
Percent Recovered
certified value
07OCT1-.521SDO
10/10/91
10/10/91
NA
58.7
20 U
N3
NS
NS
hS
NS
NS
395 315 153
NO hC ND
NS 880 NS
NS 202 NS
NS 689 NS
NS 487 NS
NS 55% NS
77.9% 123.1%
NA NA
NA NA
66.7% 100.6%
76.7% 121.3%
NA NA
NA NA
Page 1
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BUFFALO RIVER PILOT PROJECT (CF #379)
PCB/AROCLORS IN SEDIMENT SAMPLES
TABLE NO. 2
(concentrations in ng/g dry weight)
% Surrogate Recovery
MSLCode
Sponsor ID
Extraction
Date
Dry Wt.
(%)
Aroclor
1242
Aroclor
1248
Aroclor
1254
Aroclor
1260
Tetrachloro-
m-Xylene
Octachloro-
naphthalene
REPLICATE ANALYSIS
379GLBR-15, Rep 1
379GLBR-15, Rep 2
379GLBR-15, Rep 3
07OCT1:212SCO
07OCT1212SCO
070CT1212SCO
10/10/91
10/10/91
10/10/91
RSO%
59.0
59.0
59.0
73 E
79 E
73 E
5%
217
236
239
5%
99 E
108E
20 U
9%
20 U
20 U
20 U
NA
53.9%
56.8%
56.9%
NA
85.1%
89.2%
95.9%
NA
U - Not detected at detection limit shown.
E m Estimated/most likely due to residual peaks of primary aroclor.
* = Outside of laboratory control limits of 40-120%.
NA » Not Applicable.
NS m Not Spiked. NC » Not certified.
RSD % » Relative Standard Deviation.
Page 2
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